會(huì)員動(dòng)態(tài)
《分析試驗(yàn)室》2024年6月第43卷第6期中英文摘要
基于金屬有機(jī)框架材料的比率熒光印跡探針測(cè)定磺胺嘧啶
黃勇強(qiáng)1，明秦1，黃衛(wèi)紅1，楊文明*2
（1. 江蘇大學(xué)環(huán)境與安全工程學(xué)院，鎮(zhèn)江 212013；2. 江蘇大學(xué)材料科學(xué)與工程學(xué)院，鎮(zhèn)江 212013）
摘要：基于熒光分析法與分子印跡技術(shù)，構(gòu)建了一種可快速、靈敏檢測(cè)自來(lái)水和牛奶中磺胺嘧啶的熒光探針。以磺胺嘧啶為模板分子，3-氨丙基三乙氧基硅烷為功能單體，金屬有機(jī)框架材料（MOFs）為載體，將碲化鎘量子點(diǎn)（CdTe QDs）包埋于MOFs中，鎂氮共摻雜的石墨烯量子點(diǎn)（Mg，N/GQDs）為響應(yīng)信號(hào)，通過(guò)溶膠凝膠法制備了熒光分子印跡探針。對(duì)合成探針的形貌、化學(xué)結(jié)構(gòu)和性能進(jìn)行表征。結(jié)果顯示，磺胺嘧啶濃
度在0~100 μmol/L范圍內(nèi)，與熒光強(qiáng)度呈良好的線性關(guān)系，檢出限為11.23 nmol/L，回收率在96.2%~101.2%之間，相對(duì)標(biāo)準(zhǔn)偏差（RSD）小于1.7%。該探針已成功應(yīng)用于實(shí)際樣品自來(lái)水和牛奶中磺胺嘧啶的檢測(cè)。
關(guān)鍵詞：磺胺嘧啶；比率熒光；金屬有機(jī)框架；分子印跡聚合物
中圖分類號(hào)：O657.3 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0767-07
Detection for sulfadiazine by ratio fluorescent imprinting probe based on metal organic framework materials
HUANG Yongqiang1，MING Qin1，HUANG Weihong1，YANG Wenming*2
1. School of Environment and Safety Engineering，Jiangsu University，Zhenjiang 212013，China；2. School of Materials Science and Engineering，Jiangsu University，Zhenjiang 212013，China）
Abstract：Based on fluorescence analysis and molecular imprinting technology，a fluorescent probe for rapid and sensitive detection of sulfadiazine in tap water and milk was constructed. Using sulfadiazine as template molecule，3-aminopropyltriethoxysilane as functional monomer，and metal organic framework materials （MOFs） as carrier，CdTe quantum dots （CdTe QDs） were embedded in MOFs. Then，Mg and N co doped graphene quantum dots （Mg，N/GQDs） were used as response signals，and the fluorescent molecular imprinting probes were prepared by sol-gel method. The morphology，chemical structure and properties of the synthesized probe were characterized. The results showed that the concentration of sulfadiazine had a good linear relationship with fluorescence intensity in the range of 0-100 μmol/L. The detection limit was 11.23 nmol/L，the recoveries were 96.2%-101.2%，and the relative standard deviations were less than 1.7%. The probe has been successfully applied to the detection of sulfadiazine in actual samples of tap water and milk.
Keywords：sulfadiazine；ratio fluorescence；metal organic framework；molecularly imprinted polymer
反相高效液相色譜法同時(shí)拆分3種手性殺菌劑
周勵(lì)*1，唐婧2，范榮華1，陳彤1，歐陽(yáng)玉1
（1. 沈陽(yáng)醫(yī)學(xué)院公共衛(wèi)生學(xué)院，沈陽(yáng) 110034；2. 清華大學(xué)臨床醫(yī)學(xué)院，清華大學(xué)附屬北京清華長(zhǎng)庚醫(yī)院，北京 102218）
摘要：應(yīng)用Chiralpak IH手性色譜柱，建立了一種同時(shí)拆分多效唑、己唑醇、糠菌唑3種三唑類殺菌劑對(duì)映異構(gòu)體的高效液相色譜分析方法。采用反相色譜條件，以乙腈-水為流動(dòng)相，在230 nm下進(jìn)行分析，在優(yōu)化條件下，即乙腈-水（40∶60，V/V）為流動(dòng)相，柱溫35 ℃、流速1.0 mL/min時(shí)，3種三唑類殺菌劑對(duì)映異構(gòu)體能同時(shí)實(shí)現(xiàn)手性分離。
關(guān)鍵詞：高效液相色譜法；手性分離；反相；Chiralpak IH手性柱；三唑類殺菌劑
中圖分類號(hào)：TQ450.7 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0774-06
Simultaneous enantiomeric separation of three triazole fungicides by reversed-phase high performance liquid chromatography
ZHOU Li*1，TANG Jing2，F(xiàn)AN Ronghua1，CHEN Tong1，OUYANG Yu1
1. School of Public Health，Shenyang Medical College，Shenyang 110034，China；2. School of Clinical Medicine，Beijing Tsinghua Changgung Hospital，Tsinghua University，Beijing 102218，China）
Abstract：A high performance liquid chromatographic method was established for the simultaneous chiral separation of three triazole fungicides，including paclobutrazol，hexaconazole and bromuconazole with Chiralpak IH column. The analysis of three triazole fungicides was carried out by reversed-phase high performance liquid chromatography with the mobile phase of acetonitrile and water. The wavelength of UV detector was 230 nm. Under the optimized separation conditions as follows：acetonitrile-water （40∶60，V/V） as mobile phase，column temperature of 35 ℃ and flow rate of 1.0 mL/min，three triazole fungicides were chiral separated simultaneously.
Keywords：high performance liquid chromatography；chiral separation；reversed phase；Chiralpak IH column；triazole fungicide
碳點(diǎn)比率熒光探針測(cè)定果蔬中的甲胺磷
韓雍*
，汪慧，張曉燕
（隴東學(xué)院農(nóng)林科技學(xué)院，慶陽(yáng) 745000）
摘要：以鄰苯二胺與濃硫酸為原料，通過(guò)一步水熱法合成了熒光碳點(diǎn)（oPD-CDs），構(gòu)建了一種檢測(cè)果蔬中甲胺磷（MTP）的oPD-CDs比率熒光傳感器。在優(yōu)化條件下，oPD-CDs傳感器的熒光比值（F430/F483）與甲胺磷濃度在0~160 ng/mL范圍內(nèi)呈良好的線性關(guān)系，相關(guān)系數(shù)R2為0.99，檢出限（LOD）為14.3 ng/mL，加標(biāo)回收率為92.0%~108.0%，相對(duì)標(biāo)準(zhǔn)偏差（RSDs）為0.7%~1.6%。該方法可用于果蔬中甲胺磷殘留的檢測(cè)。
關(guān)鍵詞：農(nóng)藥殘留；熒光碳點(diǎn)；甲胺磷；快速檢測(cè)
中圖分類號(hào)：O657.3；O661.1 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0780-05
Carbon dots-based ratiometric fluorescent probe for the detection of methamidophos residues in fruits and vegetables
HAN Yong*，WANG Hui，ZHANG Xiaoyan
College of Agriculture and Forestry，Longdong University，Qingyang 745000，China）
Abstract：In this work，o-phenylenediamine and concentrated sulfuric acid were used as precursors to prepare multi-emissive fluorescent carbon dots （oPD-CDs） through a one-step hydrothermal method. Then，oPD-CDs were employed as a fluorescent probe for the detection of methamidophos （MTP） residues in fruits and vegetables. Under the optimal conditions，the fluorescence ratio values （F430/F483） of the oPD-CDs sensor showed a good linear relationship with the MTP concentration in the range of 0-160 ng/mL，with the correlation coefficient （R2） of 0.99. The limit of detection （LOD） was calculated as 14.3 ng/mL，the spiked recoveries were 92.0%-108.0%，and the relative standard deviations （RSDs） were 0.7%-1.6%. The method can be applied to the detection of MTP residues in fruits and vegetables.
Keywords：pesticide residues；fluorescence carbon dots；methamidophos；rapid detection
魯米諾-還原金納米粒子/碳納米管三維復(fù)合材料基電化學(xué)發(fā)光傳感器檢測(cè)血清中的乳酸
趙慧1，婁方明1，2，石曉冉1，張涵1，李群芳*1，2
（1. 湖北民族大學(xué)化學(xué)與環(huán)境工程學(xué)院，恩施 445000；2. 風(fēng)濕性疾病發(fā)生與干預(yù)湖北省重點(diǎn)實(shí)驗(yàn)室，恩施 445000）
摘要：采用一鍋水熱法制備了魯米諾-還原金納米粒子/碳納米管三維復(fù)合材料（Lu-AuNPs/CNTs），用其制備固態(tài)電化學(xué)發(fā)光（ECL）傳感器，并用于血清中乳酸的檢測(cè)。采用場(chǎng)發(fā)射掃描電子顯微鏡（FSEM）、透射電子顯微鏡（TEM）、X射線粉末衍射儀（XPS）和X射線光電子能譜儀（EDS）對(duì)Lu-AuNPs/CNTs的形貌、結(jié)構(gòu)、尺寸進(jìn)行了表征。結(jié)果表明，碳納米管（CNTs）為三維立體網(wǎng)狀結(jié)構(gòu)，魯米諾-還原金納米粒子（Lu-AuNPs）尺寸均一地分布在CNTs的表面。將Lu-AuNPs/CNTs固定在玻碳電極表面制成固態(tài)ECL傳感器，其電化學(xué)發(fā)光信號(hào)約是Lu-AuNPs的2倍。該傳感器的電化學(xué)發(fā)光強(qiáng)度與溶液中H2O2濃度成正比，線性范圍為0.5~200 μmol/L，檢測(cè)限為0.2 μmol/L。Lu-AuNPs/CNTs可用于固定乳酸氧化酶，所制備的傳感器對(duì)乳酸的檢測(cè)限為3.0 μmol/L。該生物傳感器可用于人血清樣品中乳酸的測(cè)定。
關(guān)鍵詞：一步水熱合成；魯米諾-還原金納米粒子/碳納米管三維復(fù)合材料；過(guò)氧化氫；乳酸
中圖分類號(hào)：O657.1 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0785-08
Detection of lactate in serum by electrochemiluminescence biosensor based on luminol-reduced gold nanoparticles/carbon nanotubes three dimensional nanocomposites
ZHAO Hui1，LOU Fangming1，2，SHI Xiaoran1，ZHANG Han1，LI Qunfang*1，2
1. School of Chemistry and Environmental Engineering，Hubei University for Nationalities，Enshi 445000，China；2. Hubei Provincial Key Laboratory of Rheumatic Disease Occurrence and Intervention，Enshi 445000，China）
Abstract：An electrochemiluminescence （ECL） biosensor was constructed for the detection of lactate in serum based on a new synthesized luminol-reduced gold nanoparticles/carbon nanotubes three dimensional nanocomposites （Lu-AuNPs/CNTs） synthesized by one-pot hydrothermal method. The morphology，structure，and size of Lu-AuNPs/CNTs were characterized using field emission scanning electron microscopy （FSEM），transmission electron microscopy （TEM），X-ray powder diffractometer （XPS），and X-ray photoelectron spectroscopy （EDS）. The results showed that Lu-AuNPs/CNTs had a three-dimensional network structure，and the Lu-AuNPs uniformly distributed on the surface of CNTs. A solid-state ECL sensor was constructed by fixing Lu-AuNPs/CNTs on the surface of a glassy carbon electrode，and the signal of Lu-AuNPs/CNTs was approximately twice of that of Lu-AuNPs. The ECL intensity of Lu-AuNPs/CNTs increased linearly with the increase of H2O2 concentration in the range from 0.5 to 200 μmol/L，and the limit of detection （LOD） was 0.2 μmol/L. Lactate oxidase was immobilized on Lu-AuNPs/CNTs to fabricate a lactate ECL biosensor，the LOD for lactate was 3 μmol/L. This biosensor can be used for the determination of lactate in human serum.
Keywords：one-pot hydrothermal synthesis；luminol-reduced gold nanoparticles/carbon nanotubes three dimensional nanocomposites；hydrogen peroxide；lactate
分子印跡固相萃取-高效液相色譜法檢測(cè)奶粉中3種β-興奮劑
魏盤，王建*，石雨，祁迎春，任景俞，黃華，牛志睿，孫召
（延安市環(huán)境檢測(cè)與修復(fù)重點(diǎn)實(shí)驗(yàn)室，延安大學(xué)石油工程與環(huán)境工程學(xué)院，延安 716000）
摘要：以β-興奮劑3-甲氧酪胺（3-MT）、多巴胺（DA）和去氧腎上腺素（PE）為模板，采用沉淀聚合法，分別制備了3種單模板分子印跡聚合物（SMIP）和3種混合模板分印跡聚合物（MMIP），并在水和乙醇中對(duì)其吸附和分離性能進(jìn)行了評(píng)價(jià)。結(jié)果表明，以3-MT為模板的SMIP1在乙醇中對(duì)上述3種β-興奮劑具有最佳選擇性，25 min可達(dá)吸附平衡。在對(duì)3-MT的初始濃度為0.03 mmol/L時(shí)，印跡因子（IF）最大，為2.12。SMIP1對(duì)3-MT，DA和PE的吸附量隨吸附初始濃度增加而增加，在3 mmol/L時(shí)分別達(dá)到41.26，39.83和40.47 μmol/g。以SMIP1為吸附劑從奶粉中同時(shí)高選擇性固相萃取3-MT，DA和PE，在上樣濃度為0.01，0.02和0.03 mmol/L時(shí)，高效液相色譜法（HPLC）檢測(cè)的回收率分別為98%~100%，92.5%~96%和90.3%~94%，相對(duì)標(biāo)準(zhǔn)差（RSD）分別為1.9%~5.1%，2.0%~4.0%和2.1%~4.2%。該方法適用于奶粉中3-MT的定量分析以及DA和PE的定性檢測(cè)。
關(guān)鍵詞：β-興奮劑；分子印跡聚合物；固相萃取；奶粉
中圖分類號(hào)：O657 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0793-06
Detection of three kinds of β-Agonists in milk powder by molecularly imprinted solid phase extraction-high performance liquid chromatography
WEI Pan，WANG Jian*，SHI Yu，QI Yingchun，REN Jingyu，HUANG Hua，NIU Zhirui，SUN Zhao
Key Laboratory of Environmental Testing and Restoration，School of Petroleum Engineering and Environmental Engineering，Yan'an University，Yan'an 716000，China）
Abstract：In this study，three single-template molecular imprinted polymers （SMIP） and three mixed template-molecular imprinted polymers （MMIP） were prepared by precipitation polymerization using 3-methoxytyine （3-MT），dopamine （DA） and phenylephrine （PE） as the templates，and their adsorption and separation performance were evaluated in water and ethanol. The performance tests showed that the adsorption capacity of SMIP1 with 3-MT as template had the best selectivity for the above three β-Agonists in ethanol，and the adsorption equilibrium can be reached at 25 min. When the initial concentration of 0.03 mmol/L，the imprinting factor （IF） reached the highest value of 2.12. The adsorption capacity of SMIP1 for 3-MT，DA and PE increased with the initial concentration，reaching 41.26，39.83 and 40.47 μmol/g at 3 mmol/L，respectively. The selective simultaneous extraction of 3-MT，DA and PE from milk powder were achieved by employing this SMIP1 as a solid phase extraction adsorbent. At the spiked concentrations of 0.01，0.02 and 0.03 mmol/L，the mean recoveries of 3-MT，DA and PE，as detected by high performance liquid chromatography （HPLC） method，ranged from 98% to 100%，92.5% to 96%，and 90.3% to 94%，respectively. The relative standard deviations （RSDs） ranged from 1.9% to 5.1%，2.0% to 4.0% and 2.1% to 4.2%，respectively. This method is suitable for quantitative analysis of 3-MT and qualitative detection of DA and PE in milk powder.
Keywords：β-Agonists；molecularly imprinted polymers；solid-phase extraction；milk powder
電感耦合等離子體串聯(lián)質(zhì)譜法檢測(cè)食用農(nóng)產(chǎn)品中的總溴
李愛(ài)陽(yáng)1，吳路輝1，殷子懿1，陳宇1，蔡玲1，黃建華*2
（1. 湖南工學(xué)院化學(xué)與環(huán)境工程學(xué)院，衡陽(yáng) 421002；2. 湖南省中醫(yī)藥研究院中藥研究所，長(zhǎng)沙 410013）
摘要：建立了電感耦合等離子體串聯(lián)質(zhì)譜（ICP-MS/MS）測(cè)定食用農(nóng)產(chǎn)品中總溴的方法，以N2O作為反應(yīng)氣消除質(zhì)譜干擾。在MS/MS模式下，研究了在八極桿反應(yīng)池系統(tǒng)（ORS）中N2O與Br+的相互作用?；谘踉愚D(zhuǎn)移反應(yīng)，將Br+轉(zhuǎn)移為氧化物離子BrO+，利用Br+→BrO+為離子對(duì)，消除質(zhì)譜干擾。將N2O反應(yīng)結(jié)果與采用O2的反應(yīng)結(jié)果比較，N2O能更有效地形成氧化物離子，靈敏度更高，背景等效濃度（BEC）和檢出限（LOD）更低，消除干擾更徹底。通過(guò)分析標(biāo)準(zhǔn)參考物質(zhì)，評(píng)價(jià)方法的準(zhǔn)確性和精密度，發(fā)現(xiàn)測(cè)定結(jié)果與標(biāo)準(zhǔn)參考物質(zhì)的認(rèn)證值基本一致。溴的LOD為38.4~52.6 ng/L，相對(duì)標(biāo)準(zhǔn)偏差（RSD）為1.8%~4.3%，加標(biāo)回收率在96.8%~103.0%之間。所建立的方法適用于食用農(nóng)產(chǎn)品中總溴的測(cè)定。
關(guān)鍵詞：電感耦合等離子體串聯(lián)質(zhì)譜；食用農(nóng)產(chǎn)品；總溴；N2O；氧原子轉(zhuǎn)移反應(yīng)
中圖分類號(hào)：O657.31 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0799-06
Determination of total bromine in edible agricultural products by inductively coupled plasma tandem mass spectrometry
LI Aiyang1，WU Luhui1，YIN Ziyi1，CHEN Yu1，CAI Ling1，HUANG Jianhua*2
1. Department of Chemical and Environmental Engineering，Hunan Institute of Technology，Hengyang 421002，China；2. Institute of Chinese Materia，Hunan Academy of Traditional Chinese Medicine，Changsha 410013，China）
Abstract：A new method for the determination of total bromine （Br） in edible agricultural products by inductively coupled plasma-tandem mass spectrometry （ICP-MS/MS） was established. A new strategy of using N2O as reaction gas to eliminate the spectral interference was proposed. In the MS/MS mode，the interaction between N2O and Br+ in the octopole reaction system （ORS） was studied. Based on the oxygen atom transfer reaction，Br+ was transferred to the oxide ion BrO+，and the spectral interferences were eliminated by using Br+→BrO+ as the ion pair. Comparison of the results using N2O and O2 as reaction gas revealed that N2O was more effective at forming oxides，obtaining higher sensitivity，lower background equivalent concentration （BEC） and limit of detection （LOD），and eliminating interference more thoroughly. The accuracy and precision of the method were assessed by analyzing the standard reference materials. It was found that the determination results were in good agreement with the certified values of the reference materials. The LODs of Br were 38.4-52.6 ng/L，the relative standard deviations （RSDs） were 1.8%-4.3%，and the spiked recoveries were 96.8%-103.0%. The developed analytical method is suitable for the determination of total Br in edible agricultural products.
Keywords：inductively coupled plasma tandem mass spectrometry；edible agricultural products；total bromine；N2O；oxygen atom transfer reaction
AgNPs/SiO2納米碗表面增強(qiáng)拉曼光譜基底的制備及多環(huán)芳烴檢測(cè)
王世強(qiáng)，金艷，姜慧蕓，安飛，朱亮*，肖安山
（化學(xué)品安全控制國(guó)家重點(diǎn)實(shí)驗(yàn)室，中石化安全工程研究院有限公司，青島 266100）
摘要：以膠體自組裝方法為基礎(chǔ)，制備二氧化硅（SiO2）納米碗陣列；利用多巴胺在其表面原位還原一層銀納米顆粒（AgNPs）；然后修飾一層硫醇分子，得到硫醇修飾的AgNPs/SiO2納米碗復(fù)合表面增強(qiáng)拉曼光譜（SERS）基底。通過(guò)調(diào)節(jié)AgNPs的密度和硫醇分子的種類，得到最優(yōu)化的SERS基底。該SERS基底對(duì)芘和菲的檢出限均為1×10-7 mol/L，在1×10-2~1×10-7 mol/L濃度范圍內(nèi)，拉曼信號(hào)強(qiáng)度與芘和菲濃度呈線性關(guān)系，相關(guān)系數(shù)（R2）均大于0.99。該基底具有良好的均一性和重復(fù)性，芘分子（1×10-5 mol/L）在592和1402 cm-1處拉曼信號(hào)強(qiáng)度的相對(duì)標(biāo)準(zhǔn)偏差（RSD）分別為4.0%和4.9%。該方法制備的復(fù)合SERS基底在水中痕量多環(huán)芳烴以及其他污染物的高靈敏度檢測(cè)等方面有廣闊的應(yīng)用前景。
關(guān)鍵詞：表面增強(qiáng)拉曼光譜；銀納米顆粒/二氧化硅納米碗；硫醇；疏水作用；多環(huán)芳烴
中圖分類號(hào)：O657.37 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0805-09
Fabrication of surface enhanced Raman spectroscopy substrates composed of silver nanoparticles/SiO2 nanobowls for the detection of polycyclic aromatic hydrocarbons
WANG Shiqiang，JIN Yan，JIANG Huiyun，AN Fei，ZHU Liang*，XIAO Anshan
State Key Laboratory of Safety and Control for Chemicals，SINOPEC Research Institute of Safety Engineering Co.，Ltd.，Qingdao 266100，China）
Abstract：Based on the colloidal self-assembly method，the silica （SiO2） nanobowl arrays were easily fabricated. A layer of silver nanoparticles （AgNPs） was in-situ reduced by dopamine on the surface of the nanobowls，and then the mercaptan molecules were added to fabricate mercaptan modified AgNPs/SiO2 nanobowls hierarchical surface enhanced Raman spectroscopy （SERS） substrates. The optimized SERS substrates could be obtained by adjusting the density of AgNPs and the type of mercaptan molecule. The experimental results indicated that the limits of detection of pyrene and phenanthrene by the SERS substrates were both 1×10-7 mol/L，and the linear correlation coefficients （R2） of Raman signal intensity and concentration were also above 0.99 in the concentration range of 1×10-2-1×10-7 mol/L. The SERS substrates showed excellent uniformity and repeatability. The relative standard deviations （RSDs） of the Raman signal intensity of pyrene molecules （1×10-5 mol/L） at 592 cm-1 and 1402 cm-1 were 4.0% and 4.9%，respectively. The SERS substrate prepared by this method will be applied in various application areas，such as high sensitivity detection of trace amounts of polycyclic aromatic hydrocarbons （PAHs） and other contaminants in water.
Keywords：surface enhanced Raman spectroscopy；silver nanoparticles/SiO2 nanobowls；mercaptan；hydrophobic interaction；polycyclic aromatic hydrocarbons
香豆素衍生物-紙芯片體系對(duì)3種生物硫醇的選擇性檢測(cè)
張劍，王祖黎，唐新萍，李一冰，鄭志鴻，王月萍，張博，劉春葉*
（西安醫(yī)學(xué)院藥學(xué)院，西安 710021）
摘要：合成了一種7-（二乙氨基）香豆素衍生物熒光探針，并通過(guò)紅外吸收光譜、質(zhì)譜和核磁共振波譜對(duì)其進(jìn)行結(jié)構(gòu)表征。該探針可與同型半胱氨酸（Hcy）、半胱氨酸（Cys）、谷胱甘肽（GSH）發(fā)生不同的顯色反應(yīng)，以微流控紙芯片為平臺(tái)，實(shí)現(xiàn)了對(duì)3種生物硫醇的特異性檢測(cè)。手機(jī)拍照記錄顯色結(jié)果，Photpshop軟件分析RGB通道顏色強(qiáng)度（RGB值）。當(dāng)探針濃度為10 μmol/L，3種生物硫醇濃度在10~50 μmol/L范圍內(nèi)時(shí)，RGB值與生物硫醇濃度呈良好線性關(guān)系。該方法在6 min內(nèi)即可完成實(shí)際樣品分析，結(jié)果相對(duì)誤差均小于3%，可用于疾病危險(xiǎn)因子的快速實(shí)時(shí)檢測(cè)。
關(guān)鍵詞：熒光探針；微流控紙芯片；同型半胱氨酸；半胱氨酸；谷胱甘肽
中圖分類號(hào)：O652 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0814-05
Selective detection of three biomercaptan by a coumarin derivative based paper chip
ZHANG Jian，WANG Zuli，TANG Xinping，LI Yibing，ZHENG Zhihong，WANG Yueping，ZHANG Bo，LIU Chunye*
School of Pharmacy，Xi'an Medical University，Xi'an 710021，China）
Abstract：A fluorescent probe of 7-（diethylamino） coumarin derivative was synthesized，and characterized by fourier transform infrared （FT-IR） spectroscopy，mass spectrometry （MS） and nuclear magnetic resonance （NMR） spectroscopy，respectively. This probe is capable of interacting with homocysteine （Hcy），cysteine （Cys），and glutathione （GSH） and present different colors，which supports a distinguishing detection of three biomercaptan using microfluidic paper chips as a platform. The result photos were recorded using a mobile phone，and the color intensity of RGB channel （RGB value） were assessed by Photoshop software. Favourable linear relationships were obtained between color intensity and concentrations of the three biomercaptan in the range of 10-50 μmol/L with the probe concentration of 10 μmol/L. The real sample was analyzed within 6 min，and the relative errors of the results were all less than 3%. The work demonstrates that the method is enable to be employed for rapid and real-time detection of risk factors of diseases.
Keywords：fluorescent probe；micro?uidic paper-based analytical devices；homocysteine；cysteine；glutathione
小型質(zhì)子轉(zhuǎn)移反應(yīng)質(zhì)譜儀離子源的設(shè)計(jì)與優(yōu)化
陳蹇平1，王俊1，聞路紅1，2，3，陳臘*1，2
（1. 寧波大學(xué)寧波高等技術(shù)研究院，寧波 315211；2. 寧波華儀寧創(chuàng)智能科技有限公司，寧波 315191；3. 廣州市華粵行儀器有限公司，廣州 511400）
摘要：作為一種快速、高靈敏的揮發(fā)性有機(jī)物（VOCs）檢測(cè)技術(shù)，質(zhì)子轉(zhuǎn)移反應(yīng)質(zhì)譜（PTR-MS）被越來(lái)越多地應(yīng)用于環(huán)境、醫(yī)學(xué)、公共安全等領(lǐng)域。作為PTR-MS的關(guān)鍵部件之一，空心陰極輝光放電離子源對(duì)儀器性能具有重要影響。本文通過(guò)有限元仿真優(yōu)化了空心陰極結(jié)構(gòu)，在陰極內(nèi)徑為20 mm、陽(yáng)極與陰極間隙為4 mm時(shí)，離子源放電效果較好。將優(yōu)化后的空心陰極輝光放電離子源與便攜式質(zhì)譜儀聯(lián)用，并測(cè)試了離子信號(hào)與放電氣壓和放電電流的關(guān)系。結(jié)果表明，最佳放電氣壓約為200 Pa，最佳放電電流為9~13 mA。采用乙腈樣品測(cè)試了儀器性能，系統(tǒng)響應(yīng)時(shí)間在10 s以內(nèi)，乙腈檢出限約為10-9（V/V），線性范圍為50×10-9~350×10-9 （V/V），線性相關(guān)系數(shù)R2=0.991。利用該裝置檢測(cè)了蘋果發(fā)酵過(guò)程中產(chǎn)生的VOCs隨時(shí)間的變化，證明了該儀器可用于實(shí)際樣品檢測(cè)。
關(guān)鍵詞：質(zhì)子轉(zhuǎn)移反應(yīng)質(zhì)譜；空心陰極輝光放電離子源；揮發(fā)性有機(jī)物；線性離子阱；有限元仿真
中圖分類號(hào)：O657.31；X832 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0819-09
Design and optimization of the ion source for miniature proton transfer reaction mass spectrometer
CHEN Jianping1，WANG Jun1，WEN Luhong1，2，3，CHEN La*1，2
1. Ningbo Institute of Advanced Technologies，Ningbo University，Ningbo 315211，China；2. China Innovation Instrument Co. Ltd.，Ningbo 315191，China；3. Hua Yue Enterprise Holdings Ltd.，Guangzhou 511400，China）
Abstract：As a rapid and highly sensitive technique for volatile organic compounds （VOCs） detection，proton transfer reaction mass spectrometry （PTR-MS） is increasingly used in environment，medical，and public safety fields. As a key component of PTR-MS，the hollow cathode glow discharge ion source is very important for the performance of the instrument. In this work，the hollow cathode structure was optimized by finite element simulation，and the best discharge effect had been achieved with a cathode at inner diameter of 20 mm and a gap of 4 mm between anode and cathode. The hollow cathode glow discharge ion source was coupled to a portable mass spectrometer. The effects of pressure and discharge current on ion signals were verified experimentally. The results showed that the optimum discharge pressure was about 200 Pa and the optimum discharge current was between 9 and 13 mA. The instrument performance was tested with acetonitrile samples. The results showed that the response time of the system to acetonitrile was within 10 s，the limit of detection was about 10-9（V/V），and the linearity range was 50×10-9-350×10-9 （V/V） with a correlation coefficient of R2=0.991. Finally，the device was used to detect the variation of VOCs released during apple fermentation over time，demonstrating that the instrument can be used for actual samples analysis.
Keywords：proton transfer reaction mass spectrometry；hollow cathode glow discharge ion source；volatile organic compounds；linear ion trap；finite element simulation
化學(xué)樣品前處理設(shè)備的研制及應(yīng)用
王曉香*1，時(shí)雪釗2，陳鵬飛1
（1. 冰凍圈科學(xué)國(guó)家重點(diǎn)實(shí)驗(yàn)室，中國(guó)科學(xué)院西北生態(tài)環(huán)境資源研究院，蘭州 730000；2. 蘭州大學(xué)化學(xué)化工學(xué)院，蘭州 730000）
摘要：設(shè)計(jì)開(kāi)發(fā)了一套多功能樣品前處理設(shè)備，可在線或離線完成樣品處理。該設(shè)備以電滲析原理為基礎(chǔ)，將膜交換與閥切換技術(shù)組合使用，實(shí)現(xiàn)了酸堿中和、除鹽、過(guò)濾、稀釋、濃縮、基體消除等功能。通過(guò)實(shí)驗(yàn)驗(yàn)證了儀器的可靠性和可行性。采用75 μm的樹(shù)脂和1.5 mm管徑，得到最佳中和容量；中和能力可通過(guò)調(diào)節(jié)電流大小進(jìn)行調(diào)控。飽和溶液的中和/除鹽效率達(dá)100%，2~100倍稀釋，連續(xù)8次測(cè)試的相對(duì)標(biāo)準(zhǔn)偏差（RSD）<5%；濃縮連續(xù)5次進(jìn)樣的RSD<4.5%。基體消除能力強(qiáng)，甲醇處理后可直接進(jìn)入分析儀器進(jìn)行測(cè)試。各功能可自由組合，也可連接離子色譜、等離子體質(zhì)譜等儀器，進(jìn)行在線樣品前處理；特別是設(shè)備中和單元，可在線自動(dòng)再生，彌補(bǔ)了現(xiàn)有技術(shù)的不足。該設(shè)備可廣泛應(yīng)用于食品、化工、生物、醫(yī)藥、水處理、核電、環(huán)境和材料等領(lǐng)域的樣品前處理。
關(guān)鍵詞：前處理；設(shè)備研制；電滲析；中和；應(yīng)用
中圖分類號(hào)：TH122 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0828-06
Development and application of pretreatment equipment for chemical samples
WANG Xiaoxiang*1，SHI Xuezhao2，CHEN Pengfei1
1. State Key Laboratory of Cryospheric Science，Northwest Institute of Eco-Environment and Resources，Chinese Academy of Sciences，Lanzhou 730000，China；2. College of Chemistry and Chemical Engineering，Lanzhou University，Lanzhou 730000，China）
Abstract：Based on the principle of electrodialysis，a multi-functional sample pretreatment equipment，which can complete sample processing online or offline，was designed and developed. The equipment combines membrane exchange and valve switching technology to achieve acid-base neutralization，desalination，filtration，dilution，concentration，matrix elimination and other functions. The reliability and feasibility of the instrument were verified through experiments. When using 75 μm resin and 1.5 mm pipe，the optimal neutralization capacity can be obtained for the equipment，and it can be controlled by tuning the current. The neutralization/desalination efficiency of the saturated solution reached 100%，with the relative standard deviation （RSD） less than 5% for 8 times consecutive dilutions at 2 to 100 times，and the RSD was less than 4.5% for 5 consecutive injection tests for concentration. The matrix elimination ability of this equipment is excellent，the samples can be directly fed into analysis instruments after methanol treatment. Each function can be freely combined or be connected to analytical instruments such as ion chromatography and plasma mass spectrometry for sample pre-treatment. Especially，the neutralization unit of the equipment can automatically regenerate online，which compensates for the shortcomings of existing technology. This equipment can be widely applied in sample pretreatment in food，chemical，biology，medicine，water treatment，nuclear power，environment and materials fields.
Keywords：pretreatment；equipment development；electrodialysis；neutralization；application
基質(zhì)分散固相萃取-氣質(zhì)聯(lián)用法測(cè)定皮革中12種揮發(fā)性全氟和多氟化合物
高永剛1，王巖2，李曉瞳3，牛增元*1，羅忻1，葉曦雯1，張艷艷4，鄭麗莎1，王銘1
（1. 青島海關(guān)技術(shù)中心，青島 266114；2. 山東魯檢科技有限公司，青島 266002；3. 中國(guó)海洋大學(xué)海洋環(huán)境與生態(tài)教育部重點(diǎn)實(shí)驗(yàn)室，青島 266100；4. 青島市產(chǎn)品質(zhì)量檢驗(yàn)研究院，青島 266022）
摘要：建立了分散固相萃?。?em>d-SPE）-氣相色譜-質(zhì)譜法（GC-MS）同時(shí)測(cè)定皮革中12種揮發(fā)性全氟和多氟化合物（PFAS）的方法，包括4種氟化調(diào)聚物醇（FTOHs）、3種氟調(diào)聚丙烯酸酯（FTAs）、5種全氟辛烷磺酰胺（FOSAs）?？疾炝颂崛l件、凈化方法和定容溶劑對(duì)提取效率的影響。最終確定采用10 mL乙腈為提取溶劑，50 ℃下超聲提取20 min，取1 mL提取液經(jīng)100 mg GCB分散固相萃取凈化后，GC-MS選擇離子模式（SIM）檢測(cè)，外標(biāo)法定量。結(jié)果表明：12種揮發(fā)性PFAS在0.02~5.0 mg/L范圍內(nèi)線性關(guān)系良好，相關(guān)系數(shù)（R2）均不低于0.9990；方法回收率為77.6%~110.5%，相對(duì)標(biāo)準(zhǔn)偏差（RSD）為1.5%~11%，方法定量限（LOQ）為0.2 mg/kg。該方法適用于皮革中PFAS的確證和定量分析。
關(guān)鍵詞：皮革；揮發(fā)性全氟和多氟化合物；分散固相萃??；氣相色譜-質(zhì)譜法
中圖分類號(hào)：O657.63 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0834-07
Determination of 12 volatile perfluoroalkyl and polyfluoroalkyl substances in leathers by dispersive solid-phase extraction-gas chromatography-mass spectrometry
GAO Yonggang1，WANG Yan2，LI Xiaotong3，NIU Zengyuan*1，LUO Xin1，YE Xiwen1，ZHANG Yanyan4，ZHENG Lisha1，WANG Ming1
1. Technology Center of Qingdao Customs，Qingdao 266114，China；2. Shandong Lujian Technology Co.，LTD，Qingdao 266002，China；3. Key Laboratory of Marine Environment and Ecology，Ministry of Education，Ocean University of China，Qingdao 266100，China；4. Qingdao Product Quality Testing Research Institute，Qingdao 266022，China）
Abstract：A method for the simultaneous determination of 12 perfluoroalkyl and polyfluoroalkyl substances （PFAS） in leathers by dispersive solid-phase extraction （d-SPE）-gas chromatography-mass spectrometry （GC-MS） was developed. The target compounds including 4 kinds of fluorotelomer alcohols （FTOHs），3 kinds of fluorotelomer acrylates （FTAs），and 5 kinds of fluorooctane sulfonamides（FOSAs）. The effects of the extraction conditions，purification method，solvent for constant volume on the extraction efficiency were investigated. The target compounds were extracted at 50 ℃ for 20 min with acetonitril，then 1 mL extracting solution was purified by 100 mg graphitized carbon black （GCB），subsequently detected by GC/MS in the scan ion monitoring （SIM） mode and quantified using the external standard method. The results showed that the 12 kinds of PFAS had good linear relationships in the concentration ranges of 0.02-5.0 mg/L with the correlation coefficients （R2）>0.9990. The average recoveries were in the range of 77.6%-110.5%，with relative standard deviations （RSDs） in the range of 1.5%-11%. The limits of quantification were 0.2 mg/kg. This method could meet the needs for detection of PFAS in leathers.
Keywords：leathers；perfluoroalkyl and polyfluoroalkyl substances （PFAS）；dispersive solid-phase extraction （d-SPE）；gas chromatography-mass spectrometry （GC-MS）
基于濾過(guò)型凈化的液相色譜-串聯(lián)質(zhì)譜法測(cè)定畜禽肉中89種獸藥殘留
馮月超1，王建鳳1，喬祎娜2，劉佳1，劉艷*1
（1. 北京市科學(xué)技術(shù)研究院分析測(cè)試研究所（北京市理化分析測(cè)試中心），北京市食品安全分析測(cè)試工程技術(shù)研究中心，北京 100089；2. 北京市城市學(xué)院生物醫(yī)藥學(xué)部，北京100094）
摘要：建立了一種采用濾過(guò)型凈化柱對(duì)畜禽肉樣品進(jìn)行前處理、同時(shí)測(cè)定89種獸藥殘留的液相色譜-串聯(lián)質(zhì)譜（UPLC-MS/MS）檢測(cè)方法。畜禽肉用10 mL含1% （V/V）乙酸的乙腈提取，F(xiàn)aVEx-NM柱凈化，ACQUITY BEH C18（2.1 mm×100 mm，1.7 μm）柱分離，電噴霧正、負(fù)離子模式下多反應(yīng)監(jiān)測(cè)方式（MRM）采集數(shù)據(jù)，外標(biāo)法定量。89種被測(cè)物，包括磺胺類、喹諾酮類、硝基咪唑類及其代謝物、苯并咪唑類及其代謝物、β2-興奮劑類、β-阻滯劑類、利尿劑類共7類化合物，在一定濃度范圍內(nèi)線性關(guān)系良好（R2>0.99），在雞肉、牛肉和豬肉中的加標(biāo)回收率范圍為52.3%~119.8%，相對(duì)標(biāo)準(zhǔn)偏差（RSD）均小于20%。利尿劑類的5個(gè)化合物，檢出限（LODs）范圍為0.86~4.51 μg/kg，定量限（LOQs）范圍為2.87~15.0 μg/kg，其余84個(gè)化合物的LODs范圍為0.02~0.44 μg/kg，LOQs范圍為0.07~1.48 μg/kg；LODs均滿足GB 31650-2019的要求。該方法適用于畜禽肉類中獸藥殘留的高通量快速篩查。
關(guān)鍵詞：超高效液相色譜-串聯(lián)質(zhì)譜；獸藥；畜禽肉；濾過(guò)型凈化柱
中圖分類號(hào)：TS207.5；O657.63 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0841-09
Determination of 89 kinds of veterinary drugs in livestock and poultry meat by ultra-high performance liquid chromatography-tandem mass spectrometry based on pass-through solid phase extraction purification
FENG Yuechao1，WANG Jianfeng1，QIAO Yina2，LIU Jia1，LIU Yan*1
1. Institute of Analysis and Testing，Beijing Academy of Science and Technology （Beijing Center for Physical & Chemical Analysis），Beijing Engineering Research Center of Food Safety Analysis，Beijing 100089，China；2. School of Biomedicine，Beijing City University，Beijing 100094，China）
Abstract：An ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method with a pass-through solid phase extraction （SPE） purification was developed for the determination of 89 veterinary drug residues in livestock and poultry meat simultaneously. The meat was extracted with 10 mL acetonitrile containing 1% （V/V） acetic acid，and purified by FaVEx-NM solid phase extraction column.The target analytes were separated on ACQUITY BEH C18 （2.1 mm×100 mm，1.7 μm） column，detected with electrospray ionization in the positive or negative ion mode using multiple reaction monitoring （MRM），and quantified by external standard method. The results showed that 89 kinds of veterinary drugs，including sulfonamides，quinolones，nitroimidazoles and their metabolites，benzimidazoles and their metabolites β2-stimulants，β-blockers and diuretics，had good linear relationships with the correlation coefficients （R2） higher than 0.99. The recoveries of the compounds were in the range of 52.3%-119.8% in the three matrices of chicken，pork and beef. The relative standard deviations （RSDs） were less than 20%. The limits of detections （LODs） of 5 compounds belonging to the class diuretics were 0.86-4.51 μg/kg，and the limits of quantitation （LOQs） were 2.87-15.0 μg/kg. While the LODs of the other 84 compounds were 0.02-0.44 μg/kg，and the LOQs were 0.07-1.48 μg/kg. All the LODs of the target analytes were lower than the requirements of GB 31650-2019. This method is suitable for high-throughput screening of the veterinary drug residues in livestock and poultry meat.
Keywords：ultra-high performance liquid chromatography-tandem mass spectrometry；veterinary drugs；livestock and poultry meat；pass-through solid phase extraction （pass-through SPE）
計(jì)算機(jī)輔助制備煙堿分子印跡聚合物及其在煙堿純化中的應(yīng)用
李增良，顧麗莉*，景聯(lián)鵬，唐徐禹，李國(guó)棟，楊發(fā)容
（昆明理工大學(xué)化學(xué)工程學(xué)院，昆明 650500）
摘要：基于密度泛函理論（DFT）對(duì)煙堿分子印跡聚合體系進(jìn)行輔助設(shè)計(jì)，并優(yōu)化了煙堿分子印跡聚合物（NMIPs）的制備工藝。以三氟甲基丙烯酸（TFMAA）為功能單體、乙二醇二甲基丙烯酸酯（EGDMA）為交聯(lián)劑、偶氮二異丁腈（AIBN）為引發(fā)劑，煙堿與TFMAA摩爾比為1∶3、乙腈用量為60 mL時(shí)，所得NMIPs吸附效果較優(yōu)，印跡因子為1.8。考察了NMIPs的吸附性能，并借助Scatchard模型分析發(fā)現(xiàn)：NMIPs存在高親和和低親和兩類吸附結(jié)合位點(diǎn)，最大表觀結(jié)合量為28.56 mg/g。利用所制備的NMIPs純化煙草復(fù)烤尾氣，使煙堿相對(duì)含量由63.58%上升至89.78%；經(jīng)NMIPs純化，新鮮煙葉揮發(fā)油中的煙堿相對(duì)含量由89.39%上升至95.71%。
關(guān)鍵詞：煙堿；計(jì)算機(jī)模擬；分子印跡；純化
中圖分類號(hào)：TQ314.2 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0850-08
Computer assisted preparation of nicotine molecularly imprinted polymer and its application in the purification of nicotine
LI Zengliang，GU Lili*，JING Lianpeng，TANG Xuyu，LI Guodong，YANG Farong
Faculty of Chemical Engineering，Kunming University of Science and Technology，Kunming 650500，China）
Abstract：The nicotine molecular imprinting polymerization system was designed based on the density functional theory （DFT），and the preparation process of nicotine molecular imprinting polymers （NMIPs） was optimized. Under the conditions of 2-（trifluoromethyl） acrylic acid （TFMAA） as functional monomer，ethylene glycol dimethacrylate （EGDMA） as cross-linking agent，azobisisobutyronitrile （AIBN） as initiator，the molar ratio of nicotine to TFMAA of 1∶3，and the dosage of acetonitrile of 60 mL，the prepared NMIPs had better adsorption capacity，with the imprinting factor of 1.8. The adsorption performance of NMIPs was investigated by Scatchard analysis，it indicated that there were two types of binding sites with high and low affinity of adsorption in the NMIPs，and the maximum apparent binding amount was 28.56 mg/g. When the NMIPs were used to purify nicotine from tobacco regrilling tail gas and the volatile oil of fresh tobacco leaves，the relative contents of nicotine increased from 63.58% to 89.78% and 89.39% to 95.71%，respectively.
Keywords：nicotine；computer simulation；molecular imprinting；purification
電位滴定法測(cè)定鐵中間合金中鐵含量
劉含笑1，劉凱1，王祥德1，薛婷婷1，郭飛1，呂東芹1，王巍*1，2
（1. 國(guó)合通用（青島）測(cè)試評(píng)價(jià)有限公司，青島 266000；2. 國(guó)合通用測(cè)試評(píng)價(jià)認(rèn)證股份公司，北京 101400）
摘要：建立了鐵中間合金中鐵含量測(cè)定的自動(dòng)電位滴定法，考察了溶樣體系、還原劑類型及用量、滴定環(huán)境和共存離子干擾等因素的影響。結(jié)果表明，硝酸、過(guò)氧化氫和氫氟酸對(duì)測(cè)定結(jié)果有較大的影響，在滴定前應(yīng)去除；磷酸會(huì)導(dǎo)致三氯化鈦水解，影響測(cè)定結(jié)果，應(yīng)避免引入；共存的Cr，Co和Cu等金屬離子對(duì)測(cè)定結(jié)果沒(méi)有影響。在1%~99%含量范圍內(nèi)，方法的相對(duì)標(biāo)準(zhǔn)偏差（RSD）為0.08%~0.26%。使用硅鐵、錳鐵和釹鐵硼等有證標(biāo)準(zhǔn)樣品驗(yàn)證了方法的準(zhǔn)確度。該方法解決了可視滴定方法存在的滴定終點(diǎn)顏色干擾問(wèn)題，減少了磷酸等試劑的用量，規(guī)避了分離干擾離子的復(fù)雜操作，簡(jiǎn)化了實(shí)驗(yàn)步驟，同時(shí)提高了鐵含量測(cè)定的精密度。
關(guān)鍵詞：電位滴定；中間鐵合金；鐵含量測(cè)定
中圖分類號(hào)：O655.23；TF03.1 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0858-06
Determination of iron content in intermediate ferroalloy by automatic potentiometric titration method
LIU Hanxiao1，LIU Kai1，WANG Xiangde1，XUE Tingting1，GUO Fei1，LV Dongqin1，WANG Wei*1，2
1. China United Test & Evaluation （Qingdao） Co.，Ltd.，Qingdao 266000，China；2. China United Test & Certification Co.，Ltd.，Beijing 101400，China）
Abstract：The automatic potentiometric titration method was established for the determination of iron content in intermediate ferroalloys. The factors affecting the determination results of iron content，including sample dissolving system，the type and amount of reducing agent，the titration environment and the interference of coexisting ions，were studied. The results showed that nitric acid，hydrofluoric acid，and hydrogen peroxide had great influence on the determination results，which should be removed before titration. Phosphoric acid promoted the hydrolysis of titanium trichloride affecting the determination results and should be avoided. Coexisting metal ions such as Cr，Co and Cu did not affect the determination results. Within the content range of 1%-99%，the relative standard deviations （RSDs） of the method were 0.08%-0.26%，and the accuracy of the method was verified with certified reference materials such as ferrosilicon，ferromanganese and neodymium iron boron. This method solves the problem of color interference of titration end point in visual titration method，reduces the amount of hazardous chemicals such as phosphoric acid，avoids complex operations that interfering ion separation and improves the precision of iron content determination.
Keywords：potentiometric titration；intermediate ferroalloy；iron content determination
SWCSS-DS算法在紙漿材綜纖維素近紅外分析模型傳遞中的應(yīng)用
王紅鴻1，汪瑩1，黃浩冉1，熊智新*1，胡云超1，劉智健1，梁龍2
（1. 南京林業(yè)大學(xué)輕工與食品學(xué)院，南京 210037；2. 中國(guó)林業(yè)科學(xué)研究院林產(chǎn)化學(xué)工業(yè)研究所，南京 210042）
摘要：以紙漿材為研究對(duì)象，對(duì)其綜纖維素含量模型進(jìn)行傳遞分析，以解決不同近紅外光譜儀間多元校正模型無(wú)法共享的問(wèn)題。利用篩選出儀器間具有穩(wěn)定一致光譜信號(hào)的波長(zhǎng)（SWCSS）算法，選出穩(wěn)定性較好的波長(zhǎng)，并采用直接校正法（DS）對(duì)SWCSS方法校正后仍然存在的系統(tǒng)誤差進(jìn)一步校正。該聯(lián)合算法能夠提高主機(jī)模型的普適性，降低光譜矩陣維數(shù)，使模型轉(zhuǎn)移更穩(wěn)定和簡(jiǎn)單。將本文結(jié)果與單獨(dú)的SWCSS，DS和分段直接標(biāo)準(zhǔn)化（PDS）算法校正后的傳遞結(jié)果進(jìn)行比較。結(jié)果表明，與模型傳遞前分析能力相比，SWCSS-DS聯(lián)用算法對(duì)2臺(tái)從機(jī)樣品的預(yù)測(cè)標(biāo)準(zhǔn)偏差（RMSEP）分別從2.48和2.31下降到了1.05和1.07，優(yōu)于單獨(dú)的SWCSS，DS和PDS算法結(jié)果。
關(guān)鍵詞：綜纖維素含量；近紅外光譜；穩(wěn)定一致波長(zhǎng)；DS；模型傳遞
中圖分類號(hào)：O657.63 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0864-07
Application of SWCSS-DS algorithm in the transfer of near infrared analysis model for holocellulose in pulpwood
WANG Honghong1，WANG Ying1，HUANG Haoran1，XIONG Zhixin*1，HU Yunchao1，LIU Zhijian1，LIANG Long2
1. College of Light Industry and Food Engineering，Nanjing Forestry University，Nanjing 210037，China；2. Institute of Chemical Industry of Forest Products，Chinese Academy of Forestry，Nanjing 210042，China）
Abstract：In this paper，the holocellulose content model in pulpwood was transferred and analyzed to solve the problem that the multivariate calibration models between different near-infrared spectrometers could not be shared. The wavelength with stable and consistent spectral signals （SWCSS） between the instruments algorithm was used to select the wavelength with better stability，and the direct standardization （DS） method was used to further correct the systematic errors that still exist after being corrected by the SWCSS method. The combined algorithm can improve the universality of the master model，reduce the dimension of the spectral matrix，and make the model transfer more stable and simpler. The results of this work were compared with the transfer results corrected by SWCSS，DS and piecewise direct standardization （PDS） algorithm. The results showed that the root mean squared error for prediction （RMSEP） of the SWCSS-DS combined algorithm for two slave samples decreased from 2.48 and 2.31 to 1.05 and 1.07，respectively，compared with the pre-transfer analysis ability of the model，which was better than the results of the single SWCSS，DS and PDS algorithms.
Keywords：holocellulose content；near infrared spectroscopy；stable consistent wavelength；DS algorithm；model transfer
基于分子內(nèi)電荷轉(zhuǎn)移的比率型熒光探針用于次氯酸檢測(cè)和細(xì)胞成像
張曉文*，張飛
（山西大學(xué)分子科學(xué)研究所，化學(xué)生物學(xué)與分子工程教育部重點(diǎn)實(shí)驗(yàn)室，太原 030006）
摘要：利用碳碳雙鍵（C=C）可被次氯酸（HClO）選擇性氧化的特性，研究了一種具有分子內(nèi)電荷轉(zhuǎn)移（ICT）效應(yīng)的HClO檢測(cè)熒光探針TPS。該探針由于內(nèi)部具有推拉電子結(jié)構(gòu)，探針本身在激發(fā)態(tài)下會(huì)發(fā)生ICT，發(fā)出橙紅色熒光。加入HClO后，探針?lè)肿觾?nèi)不飽和C=C被氧化成醛基，ICT效應(yīng)減弱，熒光藍(lán)移。反應(yīng)前后的光譜變化表明探針TPS可用于HClO的比率熒光檢測(cè)。選擇性實(shí)驗(yàn)表明探針TPS對(duì)HClO具有顯著的特異性識(shí)別能力。在磷酸鹽（PBS）緩沖溶液中，探針TPS對(duì)HClO的線性檢測(cè)范圍為0~80 μmol/L，檢出限為56 nmol/L。探針TPS也被證實(shí)可用于活細(xì)胞內(nèi)HClO熒光成像。
關(guān)鍵詞：熒光探針；次氯酸；分子內(nèi)電荷轉(zhuǎn)移；細(xì)胞成像
中圖分類號(hào)：O657.3 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0871-05
A ratiometric fluorescent probe based on intramolecular charge transfer for hypochloric acid detection and cell imaging
ZHANG Xiaowen*，ZHANG Fei
Key Laboratory of Chemical Biology and Molecular Engineering，Ministry of Education，Institute of Molecular Science，Shanxi University，Taiyuan 030006，China）
Abstract：A fluorescence probe TPS based on intramolecular charge transfer （ICT） effect was prepared for hypochloric acid （HClO） detection according to a mechanism that HClO is capable of selectively oxidizing the carbon-carbon double bond （C=C）. Because of the internal push-pull electronic structure，the probe TPS underwent ICT in the excited state and emitting orange-red fluorescence. After the addition of HClO，the unsaturated carbon-carbon double bond of the probe was oxidized to be aldehyde group，which weakened the ICT effect and lead to a fluorescence blue-shift. The spectral changes before and after the reaction proved that the probe TPS can be employed for the ratio detection of HClO. Moreover，the selectivity experiments demonstrated that the probe TPS possesses significant specific recognition of HClO. In PBS buffer solution，the probe TPS is capable of detecting HClO in the range of 0-80 μmol/L，with a detection limit of 56 nmol/L. Importantly，TPS can be utilized for HClO fluorescence imaging in live cells due to its low cytotoxicity.
Keywords：fluorescent probe；hypochlorous acid；intramolecular charge transfer；cell imaging
離子液體萃取-高效液相色譜法同時(shí)測(cè)定破壁靈芝孢子粉中10種三萜化合物
梁涵，張誠(chéng)賢，孫夢(mèng)瑩，成霄，吳巧攀，王新財(cái)*
（湖州市食品藥品檢驗(yàn)研究院，湖州 313000）
摘要：建立了離子液體萃取-高效液相色譜法測(cè)定破壁靈芝孢子粉中10種靈芝三萜化合物的分析方法。樣品采用液液萃取的方法，以1-丁基-3-甲基咪唑四氟硼酸鹽為分散劑，以1-己基-3-甲基咪唑六氟磷酸鹽為萃取劑提取靈芝三萜類目標(biāo)化合物，經(jīng)Shim Nex Phenyl色譜柱分離，外標(biāo)法定量。結(jié)果表明：10個(gè)三萜化合物色譜峰分離良好，在測(cè)定的質(zhì)量濃度范圍內(nèi)線性關(guān)系良好，相關(guān)系數(shù)均大于0.999，相對(duì)標(biāo)準(zhǔn)偏差（RSD）為2.3%~9.0%，實(shí)際樣品加標(biāo)回收率為77.6%~91.2%。本方法適用于靈芝三萜的定量檢測(cè)。
關(guān)鍵詞：離子液體；破壁靈芝孢子粉；萃?。混`芝三萜
中圖分類號(hào)：O657.31；X832 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0876-05
Simultaneous determination of ten triterpenoids contained in the powders of broken Ganoderma lucidum spore by high-performance liquid chromatography combined with ionic liquids extraction
LIANG Han，ZHANG Chengxian，SUN Mengying，CHENG Xiao，WU Qiaopan，WANG Xincai*
Huzhou Institute for Food and Drug Control，Huzhou 313000，China）
Abstract：A method was proposed for the simultaneous determination of ten triterpenoids in broken Ganoderma lucidum spore powders （GLSP） by combining ionic liquid extraction with high-performance liquid chromatography （HPLC）. The target Lingzhi triterpenoids were extracted through liquid-liquid extraction by taking 1-butyl-3-methylimidazolium tetrafluoroborate as dispersant and 1-hexyl-3-methylimidazolium hexafluorophosphate as extractant. Then，the extracts were separated using Shim Nex Phenyl chromatographic column and quantified by external standard method. The chromatographic peaks of ten triterpenoids were effectively separated，and the linear relationships of the ten components were satisfactory in the measured ranges of concentration. The correlation coefficients（r） exceeded 0.999，the relative standard deviations were 2.3%- 9.0%，and the average recoveries were 77.6%-91.2%. This method is suitable for the determination of triterpenoids in GLSP.
Keywords：ionic liquid；broken Ganoderma lucidum spore powders；extraction；triterpenoids
超高效液相色譜-四極桿/靜電場(chǎng)軌道阱高分辨質(zhì)譜檢驗(yàn)血和尿中的舒泰成分
張婧文1，孫鑫2，劉俊寧2，王勇2，楊瑞琴*1
（1. 中國(guó)人民公安大學(xué)偵查學(xué)院，北京 100038；2. 南京市公安局刑事科學(xué)技術(shù)研究所，南京 210001）
摘要：建立了液液萃取-超高效液相色譜-四極桿/靜電場(chǎng)軌道阱高分辨質(zhì)譜法檢驗(yàn)血和尿中的舒泰成分替來(lái)他明和唑拉西泮。以乙酸乙酯為萃取溶劑，ACQUITY UPLC BEH C18柱為分析柱，乙腈及含有0.1%甲酸和5 mmol/L甲酸銨的水為流動(dòng)相等度洗脫，在正離子模式下以全掃描-平行反應(yīng)監(jiān)測(cè)掃描模式采集分析，外標(biāo)法定量。結(jié)果表明，替來(lái)他明和唑拉西泮在0.1~50 μg/L范圍內(nèi)線性關(guān)系良好，血液和尿液中替來(lái)他明和唑拉西泮的檢出限分別為0.005，0.001 μg/L，定量限分別為0.017，0.003 μg/L。在低、中、高加標(biāo)濃度下，血液中替來(lái)他明和唑拉西泮的回收率為97.5%~105.0%，日內(nèi)相對(duì)標(biāo)準(zhǔn)偏差（RSD）為2.5%~5.7%，日間RSD為2.7%~10.4%，尿液中2種物質(zhì)的回收率為90.6%~101.2%，日內(nèi)RSD為1.2%~4.3%，日間RSD為4.2%~9.7%。該方法可用于法庭科學(xué)領(lǐng)域吸食舒泰案件中生物檢材的快速檢測(cè)。
關(guān)鍵詞：舒泰；替來(lái)他明和唑拉西泮；血液；尿液；液液萃??；超高效液相色譜-四極桿/靜電場(chǎng)軌道阱高分辨質(zhì)譜
中圖分類號(hào)：O657.7；O657.6 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0881-06
Determination of Zoletil in human blood and urine by ultra performance liquid chromatography-Q Exactive orbitrap high-resolution mass spectrometry
ZHANG Jingwen1，SUN Xin2，LIU Junning2，WANG Yong2，YANG Ruiqin*1
1. School of Criminal Investigation，People’s Public Security University of China，Beijing 100038，China；2. Institute of Forensic Science and Technology of Nanjing Public Security Bureau，Nanjing 210001，China）
Abstract：A liquid-liquid extraction-ultra performance liquid chromatography-Q Exactive orbitrap high-resolution mass spectrometry method was developed for the determination of tiletamine and zolazepam in Zoletil in blood and urine. Ethyl acetate was used as the extraction solvent，and an ACQUITY UPLC BEH C18 column was used as the analytical column. The mobile phase was consisted of acetonitrile and water containing 0.1% formic acid and 5 mmol/L ammonium formate with isocratic elution. The mass spectrometry was performed in positive ion mode under Full MS-PRM scan mode，and the quantification was calculated by the external standard method. The linearities of tiletamine and zolazepam were good in the range of 0.1-50 μg/L. The limits of detection were 0.005 and 0.001 μg/L，and the limits of quantification were 0.017 and 0.003 μg/L for tiletamine and zolazepam in blood and urine，respectively. The recoveries of tiletamine and zolazepam in blood at low，medium，and high spiked concentrations were 97.5%-105.0%，with intra-day relative standard deviations （RSDs） of 2.5%-5.7% and inter-day RSDs of 2.7%-10.4%，and the recoveries of the two substances in urine were 90.6%-101.2%，with intra-day RSD of 1.2%-4.3% and inter-day RSD of 4.2%-9.7%. The method can be used for the rapid determination of biological materials in Zoletil abuse cases in forensic science.
Keywords：Zoletil；tiletamine and zolazepam；blood；urine；liquid-liquid extraction；ultra performance liquid chromatography-Q Exactive orbitrap high-resolution mass spectrometry
在線固相萃取-超高效液相色譜-質(zhì)譜法檢測(cè)水中8種微囊藻毒素
袁東1，張恒2，張旭方1，韓聰1，徐秀麗3，柏楊巍*2，段平洲2，侯嵩*2
（1. 濱州市生態(tài)環(huán)境服務(wù)中心，濱州 256603；2. 中國(guó)環(huán)境科學(xué)研究院，國(guó)家環(huán)境保護(hù)化學(xué)品生態(tài)效應(yīng)與風(fēng)險(xiǎn)評(píng)估重點(diǎn)實(shí)驗(yàn)室，北京 100012；3. 濱州市環(huán)境保護(hù)科學(xué)技術(shù)研究所，濱州 256614）
摘要：建立了一種在線固相萃取-超高效液相色譜-質(zhì)譜同時(shí)檢測(cè)水中8種微囊藻毒素的方法。水樣經(jīng)在線富集、色譜柱分離后，梯度洗脫，采用電噴霧離子源正離子多反應(yīng)監(jiān)測(cè)模式，外標(biāo)法定量。該方法分析時(shí)長(zhǎng)為11.0 min，標(biāo)準(zhǔn)曲線的線性相關(guān)系數(shù)R2＞0.98，地表水樣品的回收率為83.8%~97.2%，相對(duì)標(biāo)準(zhǔn)偏差（RSD）為1.8%~4.9%，檢出限為0.28~0.91 ng/L。該方法適用于水體中微囊藻毒素的快速檢測(cè)。
關(guān)鍵詞：地表水；微囊藻毒素；在線固相萃??；超高效液相色譜-質(zhì)譜
中圖分類號(hào)：X832 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0887-05
Determination of 8 microcystins in water by on-line solid phase extraction coupled with ultra performance liquid chromatography-mass spectrometry
YUAN Dong1，ZHANG Heng2，ZHANG Xufang1，HAN Cong1，XU Xiuli3，BAI Yangwei*2，DUAN Pingzhou2，HOU Song*2
1. Binzhou Ecological Environment Service Center，Binzhou 256603，China；2. Chinese Research Academy of Environmental Sciences，State Environmental Protection Key Laboratory of Ecological Effect and Risk Assessment of Chemicals，Beijing 100012，China；3. Institute of Environmental Protection Science and Technology，Binzhou 256614，China）
Abstract：An online solid-phase extraction-ultra performance liquid chromatography-mass spectrometry （UPLC-MS） method was developed for the simultaneous detection of eight microcystins in water. The water samples were enriched online，separated on a chromatographic column with gradient elution，and quantified by external standard method using electrospray ionization source in positive ions multiple reaction monitoring mode. The analytical time of the method was 11.0 min，the linear correlation coefficients （R2） were higher than 0.98，the recoveries of surface water samples were 83.8%-97.2%，the relative standard deviations （RSDs） were 1.8%-4.9%，and the detection limits were 0.28-0.91 ng/L. The method is suitable for the rapid determination of microcystins in water.
Keywords：surface water；microcystin；online solid-phase extraction；ultra performance liquid chromatography-mass spectrometry
合成大麻素4CN-BINACA-ADB斑馬魚(yú)體內(nèi)代謝研究
謝宜陳，茹俊輝，周善慧，王旻昊，吳劍丙*，范一雷*
（浙江警察學(xué)院，浙江省毒品防控技術(shù)研究重點(diǎn)實(shí)驗(yàn)室，杭州 310053）
摘要：采用斑馬魚(yú)模型結(jié)合超高效液相色譜串聯(lián)四極桿-靜電場(chǎng)軌跡離子阱Q Exactive質(zhì)譜（UHPLC-Q-Obitrap-HRMS）技術(shù)，研究合成大麻素4CN-BINACA-ADB的體內(nèi)代謝途徑。結(jié)果表明，4CN-BINACA-ADB共產(chǎn)生酯水解、羧酸化、羥基化、氰基被羥基還原取代、N-烷基化等Ⅰ相代謝物11種，葡萄糖醛酸化、硫酸化等Ⅱ相代謝物3種。結(jié)合代謝物的獨(dú)特性和含量，推薦羧酸化產(chǎn)物C20H24N4O5 （M2.1）以及羧酸化和氰基還原產(chǎn)物C20H26N4O5 （M2.2）作為主要代謝標(biāo)志物。研究結(jié)果可為生物樣品中4CN-BINACA-ADB代謝物的檢驗(yàn)鑒定提供理論支撐。
關(guān)鍵詞：4CN-BINACA-ADB；合成大麻素；斑馬魚(yú)；代謝產(chǎn)物；代謝途徑
中圖分類號(hào)：O657.31；X832 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0892-08
Study on metabolites of synthetic cannabinoid 4CN-BINACA-ADB in zebrafish
XIE Yichen，RU Junhui，ZHOU Shanhui，WANG Minhao，WU Jianbing*，F(xiàn)AN Yilei*
Key Laboratory of Drug Prevention and Control Technology of Zhejiang Province，Zhejiang Police College，Hangzhou 310053，China）
Abstract：The metabolic pathway of synthetic cannabinoid 4CN-BINACA-ADB was investigated using zebrafish model combined with ultra-high performance liquid chromatography tandem quadrupole-Orbitrap high-resolution mass spectrometry （UHPLC-Q-Obitrap-HRMS）. The results showed that 4CN-BINACA-ADB produced a total of eleven metabolites of phase I include ester hydrolysis，carboxylation，N-alkylation，hydroxylation，and reduction of cyanide by hydroxyl，and three metabolites of phase II such as glucuronidation and sulfation. Relying on the uniqueness and content of metabolites，carboxylation products C20H24N4O5 （M2.1） and C20H26N4O5 （M2.2） were chosen as the main metabolic biomarkers of 4CN-BINACA-ADB in vivo. This study provides a theoretical support for inspection appraisal of 4CN-BINACA-ADB metabolites in biological samples.
Keywords：4CN-BINACA-ADB；synthetic cannabinoids；zebrafish；metabolites；metabolic pathways
Ag摻雜CuO微米管制備及氣敏性能測(cè)試
郭峰旗，孫鳳云*，張恩誠(chéng)，陸佳梁，梁衍宇
（黑龍江省微納敏感器件與系統(tǒng)重點(diǎn)實(shí)驗(yàn)室，黑龍江大學(xué)電子工程學(xué)院，哈爾濱 150080）
摘要：以脫脂棉為模板，硝酸銅為銅源，采用浸漬與燒結(jié)方法制備CuO；引入不同量的Ag修飾CuO形成Ag/CuO微米管復(fù)合結(jié)構(gòu)，用于揮發(fā)性有機(jī)物檢測(cè)。利用熱分析儀（TG）、掃描電子顯微鏡（SEM）、透射電子顯微鏡（TEM）、X射線衍射（XRD）和X射線光電子能譜（XPS）等手段分析樣品的燒結(jié)情況、表面形貌、微結(jié)構(gòu)、晶體結(jié)構(gòu)和化學(xué)成分。結(jié)果表明，所制備的CuO樣品均為單斜相，且成功復(fù)刻了脫脂棉結(jié)構(gòu)，整體呈微米管狀；引入的Ag與CuO成功復(fù)合，形成Ag/CuO微米管復(fù)合結(jié)構(gòu)。引入適當(dāng)含量Ag可有效提升CuO微米管對(duì)乙醇的檢測(cè)能力，Cu/Ag摩爾比10∶1的傳感器對(duì)100 μL/L乙醇的檢測(cè)靈敏度達(dá)14.87，響應(yīng)/恢復(fù)時(shí)間為349 s/147 s，具有良好的重復(fù)性與長(zhǎng)期穩(wěn)定性。
關(guān)鍵詞：CuO微米管；Ag；乙醇；氣敏性能
中圖分類號(hào)：TP212 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0900-06
Fabrication and gas sensing performance of Ag doped CuO microtubes
GUO Fengqi，SUN Fengyun*，ZHANG Encheng，LU Jialiang，LIANG Yanyu
Heilongjiang Provincial Key Laboratory of Micro-nano Sensitive Devices and Systems，School of Electronic Engineering，Heilongjiang University，Haerbin 150080，China）
Abstract：Taking absorbent cotton （AC） as template，Cu（NO3）2 as copper source，CuO was prepared by impregnation and sintering method，and then different amounts of Ag was added to modify CuO to achieve Ag/CuO microtubes composite structure，which can be used for the detection of volatile organic compounds. The sintering situation，morphology，microstructure，crystal structure and chemical composition were analyzed by thermogravimetric analyzer （TG），scanning electron microscope （SEM），transmission electron microscope （TEM），X-ray diffractometer （XRD） and X-ray energy spectrum （XPS）. The results showed that the prepared monoclinic CuO successfully replicated the structure of AC with a tubular structure in whole；the added Ag was successfully complexed with CuO，forming Ag/CuO microtube composite structure. Appropriate amount of Ag was introduced to effectively improve the detection ability of CuO microtubes for ethanol. At 160 ℃，the sensor with copper-silver molar ratio of 10∶1 had a sensitivity of 14.87 to 100 μL/L ethanol，with the response/recovery time of 349 s/147 s，and good repeatability and long-term stability.
Keywords：CuO microtube；Ag；ethanol；gas sensing performance
基于氮硫摻雜碳點(diǎn)黃色熒光增強(qiáng)效應(yīng)選擇性檢測(cè)環(huán)境水體中的Cu2+
張曉淳1，江曉君2，霍志銘*2
（1. 廣東省中山生態(tài)環(huán)境監(jiān)測(cè)站，中山 528400；2. 廣東藥科大學(xué)公共衛(wèi)生學(xué)院，廣州 510006）
摘要：以鄰苯二胺為氮源，硫脲為硫源，通過(guò)一步溶劑熱法合成氮硫摻雜碳點(diǎn)（NS-CDs），其熒光量子產(chǎn)率為6.9%；加入Cu2+后熒光量子產(chǎn)率躍升至45.6%，同時(shí)熒光從淡灰黃色變成強(qiáng)烈的亮黃色。基于該Off-On型熒光增強(qiáng)效應(yīng)，建立了水中Cu2+的熒光快速檢測(cè)方法，線性范圍為0.05~10.0 μmol/L，檢出限低至0.01 μmol/L。應(yīng)用于環(huán)境水體中Cu2+檢測(cè)，實(shí)際樣品加標(biāo)回收率在83.3%~115.7%之間，相對(duì)標(biāo)準(zhǔn)偏差（RSD）<7.0%。樣品測(cè)定結(jié)果與ICP-MS法結(jié)果基本一致。結(jié)合便攜LED光源，可實(shí)現(xiàn)環(huán)境水體中Cu2+的現(xiàn)場(chǎng)快速監(jiān)測(cè)。
關(guān)鍵詞：氮硫摻雜碳點(diǎn)；熒光增強(qiáng)；Cu2+；快速檢測(cè)
中圖分類號(hào)：O661.1；X832 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0906-08
Selective detection of copper ion in environmental water based on yellow fluorescence-enhanced effect of nitrogen and sulfur-doped carbon dots
ZHANG Xiaochun1，JIANG Xiaojun2，HUO Zhiming*2
1. Zhongshan Ecology and Environment Monitoring Station of Guangdong Province，Zhongshan 528400，China；2. School of Public Health，Guangdong Pharmaceutical University，Guangzhou 510006，China）
Abstract：Nitrogen and sulfur co-doped carbon dots （NS-CDs） were prepared by the one-step solvothermal synthesis method with o-phenylenediamine as nitrogen source and thiourea as sulfur source. The fluorescence quantum yield of NS-CDs was 6.9%. After adding Cu2+，the fluorescence quantum yield jumped to 45.6%，and the fluorescence changed from pale yellow to strong bright yellow. Based on the Off-On fluorescence-enhanced effect of NS-CDs，a new fluorescent method had been established for the rapid detection of Cu2+ in water in the linear range from 0.05 to 10.0 μmol/L，with the detection limit as low as 0.01 μmol/L. Furthermore，the results of NS-CDs applied for the detection of Cu2+ in environmental water were satisfied，the spiked recoveries were from 83.3% to 115.7% and the relative standard deviations （RSDs） were less than 7.0%，which were basically consistent with those of ICP-MS method. The method can be applied for rapid on-site monitoring of Cu2+ in environmental water with the help of portable LED light source.
Keywords：nitrogen and sulfur doped carbon dots；fluorescent enhancement；copper ion；rapid detection
基于成像和質(zhì)譜的流式細(xì)胞術(shù)在醫(yī)學(xué)診斷中的應(yīng)用進(jìn)展
楊瑞1，張紀(jì)媛1，于玉潔1，張順心1，王合宇1，劉大喜1，2，田亮*1，2，崔建升*1，2
（1. 河北科技大學(xué)環(huán)境科學(xué)與工程學(xué)院，石家莊 050018；2. 河北省污染防治生物技術(shù)實(shí)驗(yàn)室，石家莊 050018）
摘要：人體內(nèi)部分細(xì)胞的種類變化和生理狀態(tài)是人體健康的重要指標(biāo)，對(duì)細(xì)胞進(jìn)行生化分析是醫(yī)學(xué)診斷的重要手段?；诔上窈唾|(zhì)譜的流式細(xì)胞術(shù)，在細(xì)胞分析上具有高通量、特異性強(qiáng)的優(yōu)點(diǎn)，能夠表征人體血液或組織樣本中特定的細(xì)胞類型和形態(tài)特征，從而實(shí)現(xiàn)疾病的診斷。本文綜述了成像流式細(xì)胞術(shù)（IFC）、質(zhì)譜流式細(xì)胞術(shù)（CyTOF）和成像質(zhì)譜細(xì)胞術(shù)（IMC）在腫瘤學(xué)、免疫學(xué)、血液學(xué)等醫(yī)學(xué)領(lǐng)域中最新的應(yīng)用進(jìn)展。
關(guān)鍵詞：流式細(xì)胞術(shù)；細(xì)胞分析；生物標(biāo)志物檢測(cè)；醫(yī)學(xué)診斷
中圖分類號(hào)：O657；R446 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）06-0914-11
Application progress of imaging and mass spectrometry based flow cytometry in medical diagnosis
YANG Rui*1，ZHANG Jiyuan1，YU Yujie1，ZHANG Shunxin1，WANG Heyu1，LIU Daxi1，2，TIAN Liang*1，2，CUI Jiansheng*1，2
1. College of Environmental Science and Engineering，Hebei University of Science and Technology，Shijiazhuang 050018，China；2.Hebei Key Laboratory of Pollution Prevention Biotechnology，Shijiazhuang 050018，China）
Abstract：The variety and physiological state of some cells in human body are important indicators for human health. Hence，biochemical analysis of cells is an important method of medical diagnosis. Imaging and mass spectrometry based flow cytometry has the advantages of high throughput and specificity in cellular assays，which can characterize the types and morphological of specific cells in human blood or tissue samples to realize the disease diagnostic. Thus，this review summarizes the latest advances of imaging flow cytometry （IFC），cytometry by time-of-flight （CyTOF） and imaging mass cytometry （IMC） in oncology，immunology，and hematology.
Keywords：flow cytometry；cell analysis；biomarker detection；medical diagnosis
