會(huì)員動(dòng)態(tài)
《分析試驗(yàn)室》2024年1月第43卷第1期中英文摘要
BiOI/g-C3N4修飾電極伏安法檢測(cè)磺胺甲噁唑
武天恒，劉蕊*，韓雪，劉日嘉，孫源
（哈爾濱商業(yè)大學(xué)藥學(xué)院藥物工程技術(shù)研究中心，哈爾濱 150076）
摘要：通過(guò)熱聚合法高溫煅燒尿素得到g-C3N4納米片，再以溶劑熱法得到BiOI/g-C3N4復(fù)合材料，采用X射線衍射（XRD）、掃描電子顯微鏡（SEM）、透射電子顯微鏡（TEM）、紅外光譜（FT-IR）等手段對(duì)BiOI/g-C3N4納米復(fù)合材料的微觀結(jié)構(gòu)和形貌進(jìn)行了表征。通過(guò)滴涂法將BiOI/g-C3N4復(fù)合材料修飾在玻碳電極（GCE）表面，構(gòu)建了用于快速檢測(cè)磺胺甲噁唑（SMX）的電化學(xué)傳感平臺(tái)，通過(guò)循環(huán)伏安（CV）和差分脈沖伏安（DPV）技術(shù)對(duì)SMX進(jìn)行電化學(xué)分析，峰值電流隨SMX濃度呈線性增加，線性范圍為5~1000 μmol/L，檢出限為0.025 μmol/L。采用加標(biāo)回收法測(cè)定自來(lái)水樣品中的SMX，加標(biāo)回收率為90.0%~103.4%。
關(guān)鍵詞：g-C3N4納米片；電化學(xué)傳感器；磺胺甲噁唑
中圖分類號(hào)：O657.1；X703 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0001-08
Detection of sulfamethoxazole by cyclic voltammetric method based on BiOI/g-C3N4 modified electrode
WU Tianheng，LIU Rui*，HAN Xue，LIU Rijia，SUN Yuan
Center of Pharmaceutical Engineering and Technology，School of Pharmacy，Harbin University of Commerce，Harbin 150076，China）
Abstract：The g-C3N4 nanosheet was obtained by high-temperature calcination of urea with thermal polymerization，and the BiOI/g-C3N4 composites were obtained by a solvothermal method. The microstructure and morphology of the BiOI/g-C3N4 nanocomposites were verified by different techniques including X-ray diffraction （XRD），scanning electron microscopy （SEM），transmission electron microscopy （TEM） and infrared （FT-IR） spectroscopy. The electrochemical sensing platform for the rapid detection of sulfamethoxazole （SMX） was constructed by drop-coating the BiOI/g-C3N4 composites on the surface of a glassy carbon electrode （GCE）. SMX was detected by cyclic voltammetry （CV） and differential pulsed voltammetry （DPV），and the peak current increased linearly with SMX concentration in the linear range of 5-1000 μmol/L，with a limit of detection of 0.025 μmol/L. The spiked recoveries of SMX in tap water samples ranged from 90.0% to 103.4%.
Keywords：g-C3N4 nanosheet；electrochemical sensor；sulfamethoxazole
基于拉曼頻移的SERS分析平臺(tái)在胃癌早期診斷中的應(yīng)用研究
韋偉1，朱群山3，黃永1，石立新6，吳正3，楊永國(guó)4，劉佳2，袁夢(mèng)軒5，王震光1，蔣豐娟*2
（1. 揚(yáng)州大學(xué)附屬江都人民醫(yī)院胃腸外科，揚(yáng)州 225200；2. 揚(yáng)州大學(xué)附屬江都人民醫(yī)院消化內(nèi)科，揚(yáng)州 225200；3. 揚(yáng)州大學(xué)附屬江都人民醫(yī)院普通外科，揚(yáng)州 225200；4. 揚(yáng)州大學(xué)附屬江都人民醫(yī)院病理科，揚(yáng)州 225200；5. 揚(yáng)州大學(xué)附屬江都人民醫(yī)院放射科，揚(yáng)州225200；6. 揚(yáng)州大學(xué)附屬江都人民醫(yī)院檢驗(yàn)科，揚(yáng)州 225200）
摘要：利用界面自組裝方法制備了具有優(yōu)良均一性、穩(wěn)定性和SERS活性的金銀納米梭（Au-AgNSs）基底。通過(guò)將4-巰基苯甲酸（4-MBA）修飾在Au-AgNSs基底表面，并結(jié)合癌胚抗原（CEA）的單克隆抗體，實(shí)現(xiàn)了Au-AgNSs基底的功能化。血清樣本中CEA可被其抗體捕獲并使4-MBA發(fā)生形變，導(dǎo)致特征峰發(fā)生偏移。經(jīng)驗(yàn)證，該基于拉曼頻移的SERS分析平臺(tái)具有優(yōu)異的特異性、重復(fù)性和靈敏度，對(duì)血清中CEA的檢測(cè)限（LOD）低至1.22 pg/mL。利用其對(duì)胃癌（GC）患者和健康受試者血清中CEA的表達(dá)水平進(jìn)行測(cè)定，并與酶聯(lián)免疫吸附測(cè)定法（ELISA）結(jié)果比較。結(jié)果表明，GC患者血清CEA表達(dá)水平高于健康受試者，且2種方法結(jié)果無(wú)明顯差異。因此基于拉曼頻移的SERS分析平臺(tái)在GC診斷中具有應(yīng)用價(jià)值。
關(guān)鍵詞：拉曼頻移；表面增強(qiáng)拉曼散射；胃癌；早期診斷；生物標(biāo)志物
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）01-0009-09
Raman frequency shift-based SERS analysis platform for early diagnosis of gastric cancer
WEI Wei1，ZHU Qunshan3，HUANG Yong1，SHI Lixin6，WU Zheng3，YANG Yongguo4，LIU Jia2，YUAN Mengxuan5，WANG Zhenguang1，JIANG Fengjuan*2
1. Department of Gastrointestinal Surgery，Jiangdu People’s Hospital Affiliated to Yangzhou University，Yangzhou 225200，China；2. Department of Gastroenterology，Jiangdu People’s Hospital Affiliated to Yangzhou University，Yangzhou 225200，China；3. Department of General Surgery，Jiangdu People’s Hospital Affiliated to Yangzhou University，Yangzhou 225200，China；4. Department of Pathology，Jiangdu People’s Hospital Affiliated to Yangzhou University，Yangzhou 225200，China；5. Department of Radiology，Jiangdu People’s Hospital Affiliated to Yangzhou University，Yangzhou 225200，China；6. Department of Clinical Laboratory，Jiangdu People’s Hospital Affiliated to Yangzhou University，Yangzhou 225200，China）
Abstract：Au-AgNSs substrates with excellent uniformity，stability and SERS activity were prepared using an interface self-assembly strategy. The functionalization of Au-AgNSs substrates was achieved by modifying 4-mercaptobenzoic acid （4-MBA） onto the surface of Au-AgNSs substrates and binding the anti-CEA. CEA in serum samples can be captured by anti-CEA and deforms 4-MBA，resulting in a shift of the characteristic peak. The Raman frequency shift-based SERS platform was validated to have excellent specificity，reproducibility，and sensitivity，with the limit of detection （LOD） as low as 1.22 pg/mL for CEA in serum. The SERS analysis platform was applied for the determination of CEA expression levels in gastric cancer （GC） patients and healthy human，and compared with ELISA method. The results showed that the expression levels of CEA in GC patients were higher than those of healthy human，and there was no significant difference between the two methods. Therefore，the SERS platform based on Raman frequency shift is valuable in the diagnosis of GC.
Keywords：Raman frequency shift；surface-enhanced Raman scattering；gastric cancer （GC）；early diagnosis；biomarker
構(gòu)建電化學(xué)適配體傳感器快速檢測(cè)中藥材中的赭曲霉毒素A
范申，黃榕芬，毛偉偉，張紅艷*
（福建中醫(yī)藥大學(xué)藥學(xué)院，福州 350122）
摘要：利用殼聚糖（CS）、還原氧化石墨烯（rGO）與氮摻雜多壁碳納米管（N-MWCNTs）合成N-MWCNTs-rGO-CS復(fù)合材料，制備修飾電極，結(jié)合赭曲霉毒素A（OTA）的特異性適配體，構(gòu)建高靈敏度電化學(xué)生物傳感器，并用于中藥中OTA的含量測(cè)定。在最優(yōu)條件下，峰電流變化值與OTA濃度對(duì)數(shù)值的線性響應(yīng)范圍為2.3 pmol/L~2.3 nmol/L，檢測(cè)限為0.53 pmol/L。應(yīng)用該方法對(duì)中藥飲片中OTA的含量進(jìn)行加標(biāo)回收實(shí)驗(yàn)，回收率在97.6%~103.2%之間。該方法有望用于中藥材中OTA污染的快速檢測(cè)。
關(guān)鍵詞：赭曲霉毒素A；電化學(xué)適配體傳感；快速檢測(cè)；中藥材
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）01-0018-06
Construction of electrochemical aptamer sensor for rapid detection of OTA in Chinese herbal medicine
FAN Shen，HUANG Rongfen，MAO Weiwei，ZHANG Hongyan*
Pharmacy College of Fujian University of Traditional Chinese Medicine，F(xiàn)uzhou 350122，China）
Abstract：An electrochemical biosensor was constructed based on specific aptamer for the rapid detection of ochratoxin A （OTA） in Chinese herbal medicine. The modified electrode was prepared by N-MWCNTs-rGO-CS composites consisting of chitosan （CS），reduced graphene oxide （rGO） and nitrogen-doped multi-walled carbon nanotubes （N-MWCNTs）. Under the optimal conditions，a linear response range between the logarithm of OTA concentration and peak current change was 2.3 pmol/L-2.3 nmol/L，and the detection limit was 0.53 pmol/L. This method was used to detect the content of OTA in Chinese herbal decoction pieces，and the recoveries of the standard addition were 97.6%-103.2%. This method is expected to be used for the rapid detection of OTA in Chinese herbal medicine.
Keywords：ochratoxin A；electrochemical biosensor；rapid detection；Chinese herbal medicine
基于羧基化單壁碳納米角的熒光傳感體系檢測(cè)胰蛋白酶
馮婷婷1，閆姝竹1，馬洪志1，楊麗霞1，王曉華*2
（1. 山西中醫(yī)藥大學(xué)中藥與食品工程學(xué)院，晉中 030619；2. 桂林醫(yī)學(xué)院藥學(xué)院，桂林 541004）
摘要：構(gòu)建了一種基于羧基化單壁碳納米角 （oxSWCNHs）的簡(jiǎn)單、靈敏的熒光傳感體系用于胰蛋白酶的檢測(cè)。實(shí)驗(yàn)中合成了水溶性的oxSWCNHs，并設(shè)計(jì)了一段羧基熒光素（FAM）標(biāo)記肽段作為胰蛋白酶的底物，該底物能與胰蛋白酶進(jìn)行特異性反應(yīng)。當(dāng)體系中沒(méi)有胰蛋白酶存在時(shí)，F(xiàn)AM標(biāo)記的肽段可以被oxSWCNHs強(qiáng)烈吸附，致使體系具有較低的熒光背景；當(dāng)體系中有胰蛋白酶存在時(shí)，胰蛋白酶可以與其底物肽段發(fā)生特異性水解反應(yīng)，導(dǎo)致FAM標(biāo)記的肽段水解為單個(gè)氨基酸，致使FAM遠(yuǎn)離oxSWCNHs表面，F(xiàn)AM熒光不能被oxSWCNHs淬滅，體系具有較強(qiáng)的熒光強(qiáng)度，從而實(shí)現(xiàn)熒光傳感體系對(duì)胰蛋白酶的檢測(cè)。該傳感體系線性范圍為0~2.5 μg/mL，可用于尿液中胰蛋白酶的測(cè)定。
關(guān)鍵詞：?jiǎn)伪谔技{米角；熒光傳感體系；胰蛋白酶
中圖分類號(hào)：O657.39 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0024-06
A fluorescence sensing system for the detection of trypsin based on carboxylic group-functionalized single-walled carbon nanohorns
FENG Tingting1，YAN Shuzhu1，MA Hongzhi1，YANG Lixia1，WANG Xiaohua*2
1. College of Traditional Chinese Medicine and Food Engineering，Shanxi University of Chinese Medicine，Jinzhong 030619，China；2. Pharmacy School of Guilin Medical University，Guilin 541004，China）
Abstract：A simple fluorescent sensing system for the detection of trypsin by assembling a dye-labeled peptide with carboxylic group-functionalized single-walled carbon nanohorns （oxSWCNHs） was constructed. oxSWCNHs was prepared by nitric acid oxidation of single-walled carbon nanohorn，and the carboxyfluorescein （FAM） labeled peptide （FAM-RRRRRR） was chosen as a trypsin-sensitive core substrate，which can react specific with trypsin. Without the trypsin in the system，F(xiàn)AM-labeled peptide could be strongly adsorbed by oxSWCNHs，resulting in a low fluorescence background of the system. The system reacted with trypsin to cleave the peptide，resulting in the release of the dye moiety and a substantial increase in fluorescence intensity，and trypsin could be quantified accordingly. The linear range of the system was 0-2.5 μg/mL，and the method can be applied to detect trypsin in urine samples.
Keywords：single-walled carbon nanohorns；fluorescence sensing system；trypsin
基于量子點(diǎn)微球免疫層析法快速靈敏檢測(cè)雞肉中甲氧芐啶
謝敏1，費(fèi)丹1，徐俊1，賴科洋2，陳媛3，羅凱3，彭娟4，周瑤敏*1
（1. 農(nóng)業(yè)農(nóng)村部禽類產(chǎn)品質(zhì)量安全控制重點(diǎn)實(shí)驗(yàn)室，江西省農(nóng)業(yè)科學(xué)院農(nóng)產(chǎn)品質(zhì)量安全與標(biāo)準(zhǔn)研究所，南昌 330200；2. 荷蘭瓦赫寧根大學(xué)及研究中心，瓦赫寧根 6700AA；3. 江西維邦生物科技有限公司，南昌 330029；4. 南昌大學(xué)食品科學(xué)與技術(shù)國(guó)家重點(diǎn)實(shí)驗(yàn)室，南昌 330047）
摘要：建立了一種快速靈敏檢測(cè)甲氧芐啶的量子點(diǎn)微球免疫層析法，對(duì)pH、標(biāo)記抗體濃度、試紙條檢測(cè)線上的抗原濃度以及試紙條結(jié)合墊上的探針體積進(jìn)行了優(yōu)化。通過(guò)量子點(diǎn)微球試紙條檢測(cè)儀讀取試紙條上檢測(cè)線和質(zhì)控線的熒光信號(hào)強(qiáng)度，以甲氧芐啶的濃度為橫坐標(biāo)，檢測(cè)線和質(zhì)控線熒光信號(hào)強(qiáng)度的比值為縱坐標(biāo)，建立標(biāo)準(zhǔn)曲線。結(jié)果表明，方法定量檢測(cè)范圍為1~32 μg/L，半抑制率為3.3 μg/L，回收率在99.8%~117.4%之間，與12種磺胺類藥物均只有不到2%的交叉反應(yīng)率。該方法適合大批量樣品的現(xiàn)場(chǎng)篩查。
關(guān)鍵詞：量子點(diǎn)微球；甲氧芐啶；檢測(cè)；免疫層析法
中圖分類號(hào)：O657.6 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0030-06
Quantum dots-based lateral flow assay for the rapid and sensitive detection of trimethoprim in chicken muscle
XIE Min1，F(xiàn)EI Dan1，XU jun1，LAI Keyang2，CHEN Yuan3，LUO Kai3，PENG Juan4，ZHOU Yaomin*1
1. Key Laboratory for Quality and Safety Control of Poultry Products，Ministry of Agriculture and Rural Affairs of the People's Republic of China，Institute for Quality & Safety and Standards of Agricultural Products Research，Jiangxi Academy of Agricultural Sciences，Nanchang 330200，China；2. Wageningen University and Research Centre，Wageningen 6700AA，Netherlands；3. Jiangxi Weibang Biotechnology Co.，Ltd.，Nanchang 330029，China；4. State Key Laboratory of Food Science and Technology，Nanchang University，Nanchang 330047，China）
Abstract：A method for rapid and sensitive detection of trimethoprim by the quantum dot nanobeads （QBs）-based lateral flow assay was developed. Four parameters were optimized，including pH，the concentration of antibody used for labeling，the concentration of the antigen sprayed on the test line，and the volume of antibody-QB probe on the conjugated pad. With a quantum dot strip reader，the fluorescence signal intensities of the test line （T） and control line （C） on the lateral flow strip were recorded. The standard curve was established by plotting the T/C ratio against the concentration of trimethoprim. This assay showed a good linear range from 1 to 32 μg/L and a half inhibition rate of 3.3 μg/L. The recoveries of this assay ranged from 99.8% to 117.4%，the cross-reactivity of this assay with twelve sulfonamides was less than 2%. This method could be used for screening a large batch of samples on site.
Keywords：quantum dot nanobeads；trimethoprim；detection；immunochromatography
Toehold鏈置換輔助智能手機(jī)比色法特異性檢測(cè)廢水中新冠病毒靶標(biāo)RNA
張琳，張穎，宋九華，韓耀霞，楊孝容，雷欣夢(mèng)，黃莉翔，徐君茹，何思儀，邱小鳳，史鎧*
（樂(lè)山師范學(xué)院新能源材料與化學(xué)學(xué)院，樂(lè)山 614000）
摘要：基于Toehold介導(dǎo)的鏈置換反應(yīng)（TSDR）與DNA酶，構(gòu)建了一個(gè)強(qiáng)特異性及低成本檢測(cè)廢水中SARS-CoV-2靶標(biāo)RNA單堿基突變的比色生物傳感器。SARS-CoV-2靶標(biāo)RNA與雙鏈DNA（dsDNA）引發(fā)TSDR，釋放出完整的G-四鏈體序列并與氯化血紅素（Hemin）結(jié)合，形成G-四鏈體/Hemin DNA酶，進(jìn)而催化雙氧水氧化3，3’，5，5’-四甲基聯(lián)苯胺，使溶液呈藍(lán)色。當(dāng)SARS-CoV-2靶標(biāo)RNA存在單堿基突變時(shí)，TSDR被抑制，導(dǎo)致裸眼觀察到的溶液顏色與未突變異的靶標(biāo)相比更淺。同時(shí)采用智能手機(jī)攝像頭捕捉溶液的RGB值變化（ΔRGB），對(duì)裸眼觀察結(jié)果的準(zhǔn)確性進(jìn)行驗(yàn)證。在最優(yōu)條件下，構(gòu)建的比色生物傳感器能夠特異性識(shí)別單個(gè)堿基突變的SARS-CoV-2靶標(biāo)RNA，具有用于廢水中SARS-CoV-2變異毒株檢測(cè)的潛力。
關(guān)鍵詞：新冠病毒靶標(biāo)RNA；Toehold鏈置換；智能手機(jī)；廢水
中圖分類號(hào)：O654.2 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0036-06
Toehold-mediated strand displacement reaction assisted smart phone colorimetry for specific detection of SARS-CoV-2 RNA in wastewater
ZHANG Lin，ZHANG Ying，SONG Jiuhua，HAN Yaoxia，YANG Xiaorong，LEI Xinmeng，HUANG Lixiang，XU Junru，HE Siyi，QIU Xiaofeng，SHI Kai*
College of New Energy Materials and Chemistry，Leshan Normal University，Leshan 614000，China）
Abstract：A colorimetric biosensor based on toehold-mediated strand displacement reaction （TSDR） and DNAzyme with high specificity and low cost was constructed to detect single base mutation of SARS-CoV-2 target RNA in wastewater. The SARS-CoV-2 target RNA could bind to the toehold region of the DNA1/DNA2 duplex，and displace the DNA1 through TSDR，followed by liberating the pre-blocked G-quadruplex sequence，which could associate with Hemin to form G-quadruplex/Hemin DNAzyme. Subsequently，the G-quadruplex/Hemin DNAzyme could catalyze H2O2 to oxide the TMB efficiently，and change the colorless solution to be blue. However，the TSDR procedure could be inhibited when a single base was mutational in the target RNA. This resulted in a lighter color of the solution. Meanwhile，a smartphone was employed to capture the change of RGB value of the solution to verify the accuracy of the measurement results. Under the optimal conditions，the developed biosensor could specifically identify SARS-CoV-2 target RNA with a single base mutation，and has an application prospect for the detection of SARS-CoV-2 variants in wastewater.
Keywords：SARS-CoV-2 target RNA；toehold-mediated strand displacement；smart phone；wastewater
己烯雌酚分子印跡聚合物的合成及吸附性
才旭紅1，劉俊渤*1，唐珊珊2，梁大棟1，靳瑞發(fā)3
（1. 吉林農(nóng)業(yè)大學(xué)資源與環(huán)境學(xué)院，長(zhǎng)春 130118；2. 秸稈綜合利用與黑土保護(hù)教育部重點(diǎn)實(shí)驗(yàn)室，吉林農(nóng)業(yè)大學(xué)生命科學(xué)學(xué)院，長(zhǎng)春 130118；3. 赤峰學(xué)院化學(xué)化工學(xué)院，赤峰 024000）
摘要：以己烯雌酚（DES）為印跡分子，甲基丙烯酸（MAA）為功能單體，采用沉淀聚合法制備了DES分子印跡聚合物（DES-MIPs）。采用密度泛函理論LC-ωPBE/6-31G（d，p）方法，模擬優(yōu)化DES 和MAA作用的摩爾比例，并考察了DES印跡作用的機(jī)理。通過(guò)靜態(tài)吸附、動(dòng)態(tài)吸附、選擇吸附、競(jìng)爭(zhēng)吸附方法考察了DES-MIPs的親和性與選擇性。結(jié)果表明：DES與MAA之間通過(guò)氫鍵相互作用，當(dāng)DES與MAA摩爾比為1∶5時(shí)，形成DES-MAA有序排列的復(fù)合物氫鍵數(shù)目最多（9），結(jié)合能最低（-146.62 kJ/mol）。該條件下制備的DES-MIPs對(duì)DES的最大吸附量為60.17 mg/g，且其動(dòng)力學(xué)吸附符合準(zhǔn)二級(jí)動(dòng)力學(xué)模型。在一元及二元吸附體系中，DES-MIPs對(duì)DES都具有優(yōu)異的選擇吸附性。
關(guān)鍵詞：己烯雌酚；甲基丙烯酸；分子印跡聚合物；模擬；吸附性
中圖分類號(hào)：O641.3 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0042-09
Study on synthesis and adsorbability of diethylstilbestrol molecularly imprinted polymers
CAI Xuhong1，LIU Junbo*1，TANG Shanshan2，LIANG Dadong1，JIN Ruifa3
1. College of Resource and Environment，Jilin Agricultural University，Changchun 130118，China；2. Key Laboratory of Straw Comprehensive Utilization and Black Soil Conservation，The Ministry of Education，College of Life，Jilin Agricultural University，Changchun 130118，China；3. College of Chemistry and Chemical Engineering，Chifeng University，Chifeng 024000，China）
Abstract：Diethylstilbestrol （DES） and methacrylic acid （MAA） were respectively empolyed as the imprinting molecule and functional monomer to prepare the DES molecularly imprinted polymers （DES-MIPs）using precipitation polymerization method. The molar ratio of DES to MAA was simulated and optimized using LC-ωPBE/6-31G（d，p） methodm and the imprinting action was explored. The affinity and selectivity of DES-MIPs were analyzed by static adsorption，dynamic adsorption，selective adsorption，and competitive adsorption. The results showed that DES interacts with MAA through hydrogen bonds. When the molar ratio of DES to MAA was 1∶5，the formed DES-MAA ordered complex possessed the largest amount of hydrogen bonds （9） and the lowest binding energy （-146.62 kJ/mol）. The maximum adsorption capacity of DES-MIPs to DES was about 60.17 mg/g under the present condition. The adsorption of DES-MIPs to DES is consistent with the quasi-secondary kinetic model. The selective adsorption of DES-MIPs to DES are excellent both in single and binary adsorption systems.
Keywords：diethylstilbestrol；methacrylic acid；molecularly imprinted polymers；simulation；adsorption property
超高效液相色譜-串聯(lián)質(zhì)譜法測(cè)定化妝品中5種免疫抑制劑
吳姣嬌1，劉玉玲1，涂曉琴1，殷帥1，李啟艷2，黃海萍*1
（1. 湖南省藥品檢驗(yàn)檢測(cè)研究院，湖南省藥品質(zhì)量評(píng)價(jià)工程技術(shù)研究中心，長(zhǎng)沙 410001；2. 山東省食品藥品檢驗(yàn)研究院，濟(jì)南 250101）
摘要：建立并驗(yàn)證了超高效液相色譜-串聯(lián)質(zhì)譜法（UHPLC-MS）同時(shí)測(cè)定化妝品中他克莫司、吡美莫司、依維莫司、西羅莫司、環(huán)孢菌素A這5種免疫抑制劑的方法。樣品采用甲醇超聲提取，Atlantis dC18 （100 mm× 2.1 mm，2 μm）色譜柱分離，0.1%乙酸-5 mmol/L乙酸銨水溶液和0.1%乙酸-5 mmol/L乙酸銨甲醇溶液為流動(dòng)相，多反應(yīng)監(jiān)測(cè)模式下測(cè)定，外標(biāo)法定量。結(jié)果表明，這5種免疫抑制劑在0.5~100 ng/mL濃度范圍內(nèi)線性關(guān)系良好，方法檢出限均低于10 ng/g，在不同化妝品基質(zhì)中低、中、高3個(gè)濃度水平的加標(biāo)回收率為93.3%~117.4%，相對(duì)標(biāo)準(zhǔn)偏差（RSD）為0.4%~7.5%。日內(nèi)RSD為2.4%~8.4%，日間RSD為3.9%~26%。該方法彌補(bǔ)了化妝品中非法添加違禁物質(zhì)檢測(cè)方法的缺失，為化妝品日常監(jiān)管提供技術(shù)支撐。
關(guān)鍵詞：免疫抑制劑；化妝品；超高效液相色譜-串聯(lián)質(zhì)譜
中圖分類號(hào)：TQ658.2 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0051-06
Quantitative determination of five immunosuppressants in cosmetics by ultra high-performance liquid chromatography-tandem mass spectrometry
WU Jiaojiao1，LIU Yuling1，TU Xiaoqin1，YIN Shuai1，LI Qiyan2，HUANG Haiping*1
1. Hunan Institute for Drug Control，Hunan Engineering & Technology Research Center for Pharmaceutical Quality Evaluation，Changsha 410001，China；2. Shandong Institute for Food and Drug Control，Jinan 250101，China）
Abstract：An ultra high-performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） method for simultaneous determination of five immunosuppressants in cosmetics，including tacrolimus，pimeclimus，everolimus，sirolimus and cyclosporine A，was established and verified. The samples were ultrasound extracted by methanol and separated by an Atlantis dC18 column （100 mm×2.1 mm，2 μm）. The mobile phases were 0.1% acetic acid-5 mmol/L ammonium acetate solution and 0.1% acetic acid-5 mmol/L ammonium acetate methanol solution. The target components were quantified by external standard method under positive ion electrospray ionization and multiple reaction monitoring （MRM） mode. The results showed that the five immunosuppressants had good linear relationships in the concentration ranges of 0.5-100 ng/mL，and the detection limits were all lower than 10 ng/g. The recoveries of the five immunosuppressants at three levels of low，medium and high concentrations in different cosmetic substrates were 93.3%-117.4% and the relative standard deviations （RSDs） were 0.4%-7.5%. The intra-day RSDs were 2.4%-8.4%，and the inter-day RSDs were 3.9%-26%. The method makes up for the lack of detection methods for illegal additives in cosmetics，and provides technical support for the daily supervision of cosmetics.
Keywords：immunosuppressant；cosmetics；ultra high-performance liquid chromatography-tandem mass spectrometry
新型靛紅腙類合成大麻素質(zhì)譜裂解規(guī)律研究
范一雷1，陳顯鑫2，薛錦鋒3，吳昊4，柯星1，徐雨*2
（1. 浙江省毒品防控技術(shù)研究重點(diǎn)實(shí)驗(yàn)室，浙江警察學(xué)院，杭州 310053；2. 浙江省禁毒和毒情監(jiān)測(cè)關(guān)鍵技術(shù)研究重點(diǎn)實(shí)驗(yàn)室，國(guó)家毒品實(shí)驗(yàn)室浙江分中心，杭州 310053；3. 嘉興市公安局，嘉興 314015；4. 浙江迪安司法鑒定中心，杭州 310007）
摘要：研究了新型靛紅腙類合成大麻素在電子轟擊（EI）和電噴霧（ESI）電離模式下的質(zhì)譜裂解規(guī)律，并建立了可疑物中該類合成大麻素的鑒定方法。采用氣相色譜-質(zhì)譜聯(lián)用（GC-MS）和液相色譜-高分辨質(zhì)譜聯(lián)用（LC-Q-Orbitrap/MS）技術(shù)，對(duì)5種新型靛紅腙類合成大麻素（MDA-19 （BZO-HEXOXIZID），5C-MDA-19 （Pentyl MDA-19，BZO-POXIZID），CHM-MDA-19 （BZO-CHMOXIZID），4en-pentyl MDA-19 （BZO-4en-POXIZID），5F-MDA-19 （5F-BZO-POXIZID））的主要碎片離子和碎裂過(guò)程進(jìn)行分析，并對(duì)獲得的質(zhì)譜圖進(jìn)行解析，推測(cè)該類合成大麻素的EI-MS及ESI-MSn碎裂規(guī)律。EI-MS可獲得比ESI-MSn更多的碎片離子用于該類合成大麻素的結(jié)構(gòu)推斷。碎片離子6，7和8對(duì)應(yīng)的質(zhì)荷比（m/z）118 （C8H8N+），132 （C8H6NO+）和146 （C8H6N2O?+）為2-氧代吲哚母核的特征碎片離子。經(jīng)酰胺鍵斷裂（碎裂途徑i）生成碎片離子1（m/z 105，C7H5O+），以及通過(guò)腙鍵及N1與側(cè)鏈之間發(fā)生斷裂（碎裂途徑iv）生成碎片離子8（m/z 146，C8H6N2O?+），可用于確定該類合成大麻素N8'位上取代基和N1末端取代側(cè)鏈。本研究闡述了5種新型靛紅腙類合成大麻素的質(zhì)譜裂解規(guī)律，并根據(jù)獲得的質(zhì)譜裂解規(guī)律建立了可疑物中該類合成大麻素的鑒定方法，為其快速結(jié)構(gòu)鑒定提供依據(jù)。
關(guān)鍵詞：靛紅腙類合成大麻素；質(zhì)譜裂解規(guī)律；快速篩查；電子轟擊質(zhì)譜；電噴霧質(zhì)譜
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）01-0057-07
Investigation of mass spectrometry-based fragmentation patterns of new “OXIZID” synthetic cannabinoids
FAN Yilei1，CHEN Xianxin2，XUE Jinfeng3，WU Hao4，KE Xing1，XU Yu*2
1. Key Laboratory of Drug Prevention and Control Technology of Zhejiang Province，Zhejiang Police College，Hangzhou 310053，China；2. Key Laboratory of Drug Monitoring and Control of Zhejiang Province，National anti-Drug Laboratory Zhejiang Regional Center，Hangzhou 310053，China；3. Jiaxing Public Security Bureau，Jiaxing 314015，China；4. Zhejiang Dian Regional Forenic Science Institute，Hangzhou 310007，China）
Abstract：The mass spectrometry-based fragmentation patterns of new “OXIZIDs” （N-alkylisatin-acylhydrazones） synthetic cannabinoids under electron ionization （EI） and electrospray ionization （ESI） modes were investigated，and the identification method for this kind of synthetic cannabinoids in the suspicious material was developed. Gas chromatography-mass spectrometry （GC-MS） and liquid chromatography high-resolution mass spectrometry （LC-Q-Orbitrap/MS） were used to analyze five new “OXIZID”synthetic cannabinoids，including MDA-19 （BZO-HEXOXIZID），5C-MDA-19 （Pentyl MDA-19，BZO-POXIZID），CHM-MDA-19 （BZO- CHMOXIZID），4en-pentyl MDA-19 （BZO-4en-POXIZID） and 5F-MDA-19 （5F-BZO-POXIZID. The obtained mass spectra of EI-MS and ESI-MSn were analyzed and the fragmentation patterns of “OXIZID” synthetic cannabinoids were speculated. The results showed that the EI-MS could obtain more fragment ions than that of the ESI-MSn for structural identification of “OXIZID”synthetic cannabinoids. The fragment ions 6，7 and 8 correspond to mass-to-charge ratios of 118 （C8H8N+），132 （C8H6NO+） and 146 （C8H6N2O?+），respectively，which are characteristic fragment ions of the 2-oxoindole parent nucleus. Fragment ions 1 （m/z 105，C7H5O+） and 8 （m/z 146，C8H6N2O?+），generated through the cleavage of amide bond （fragmentation pathway i），hydrazone bonds and the bond between N1 and side chains （fragmentation pathway iv），respectively，can be applied to infer the N8' position substituent and the N1 terminal substitution side chain of “OXIZID” synthetic cannabinoids. The results elucidated the mass spectrometry fragmentation patterns of new “OXIZID” synthetic cannabinoids. And the identification method for this kind of synthetic cannabinoids in the suspicious material was developed based on the obtained EI-MS and ESI-MSn fragmentation patterns of “OXIZID”synthetic cannabinoids，which could provide a basis for their rapid structural identification their.
Keywords：“OXIZID”synthetic cannabinoids；fragmentation patterns；rapid screen；EI-MS；ESI-MSn
聚β-環(huán)糊精修飾電極零流電位法檢測(cè)氯吡脲
馬明明*1，何成毅2，史帥1，崔淑慧1，劉佳1
（1. 西安工程大學(xué)環(huán)境與化學(xué)工程學(xué)院，西安 710048；2. 西安市農(nóng)產(chǎn)品質(zhì)量安全檢驗(yàn)監(jiān)測(cè)中心，西安 710077）
摘要：采用電聚合方法，在多壁碳納米管修飾的鉛筆芯電極（MWCNT-PEC）表面制備聚β-環(huán)糊精-氯吡脲（CPPU）復(fù)合材料（P-β-CD-CPPU），并對(duì)其結(jié)構(gòu)和形貌進(jìn)行表征。結(jié)果表明，含有CPPU分子殘留活性點(diǎn)的P-β-CD-CPPU擁有較大筒腔結(jié)構(gòu)，能重新包合識(shí)別CPPU分子，據(jù)此建立了P-β-CD-CPPU修飾電極零流電位法檢測(cè)CPPU的新方法。考察了影響P-β-CD-CPPU重新包合CPPU前后零流電位差值變化的條件。在優(yōu)化條件下，修飾電極的零流電位與CPPU濃度在0.5~50 μmol/L范圍內(nèi)成正比，CPPU的檢出限為21.4 nmol/L。CPPU體系可能共存的有機(jī)物及金屬離子均不干擾測(cè)定；同一根修飾電極對(duì)同一濃度CPPU零流電位測(cè)定值在14 d內(nèi)的相對(duì)標(biāo)準(zhǔn)偏差（RSD）為2.0%；5根不同批次修飾電極的零流電位測(cè)定值的RSD為1.7%。應(yīng)用本方法檢測(cè)實(shí)際獼猴桃樣品中CPPU殘留濃度，平均回收率為102.7%~109.1%，與液相色譜-質(zhì)譜聯(lián)用法檢測(cè)結(jié)果基本一致。
關(guān)鍵詞：氯吡脲；零流電位法；β-環(huán)糊精；電聚合；超分子識(shí)別
中圖分類號(hào)：O657.1；O625.63 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0064-06
Determination of forchlorfenuron by zero current potentiometry using poly-β-cyclodextrin modified electrode
MA Mingming*1，HE Chengyi2，SHI Shuai1，CUI Shuhui1，LIU Jia1
1. School of Environmental and Chemical Engineering，Xi’an Polytechnic University，Xi’an 710048，China；2. Center for Quality and Safety Inspection and Testing of Agricultural Products of Xi’an City，Xi’an 710077，China）
Abstract：Poly β-cyclodextrin-forchlorfenuron composite （P-β-CD-CPPU） was prepared using electropolymerization on the surface of a pencil core electrode modified by multiwalled carbon nanotubes （MWCNT-PEC）. The structure and surface morphology were characterized. The results showed that P-β-CD-CPPU has a much larger tube structure with active sites of forchlorfenuron residue，which could recognize and include forchlorfenuron again. A new method for the determination of forchlorfenuron was established based on this mechanism. All conditions for the detection of forchlorfenuron with the P-β-CD-CPPU modified electrode were investigated. Under the optimal conditions，the zero potential of the modified electrode had a linear relationship with forchlorfenuron concentrations in the range of 0.5-50 μmol/L. The detection limit was 21.4 nmol/L. The possible coexisting organic compounds and metal ions in the CPPU system did not interfere with the determination. The relative standard deviation （RSD） of the zero current potential of the same CPPU concentration was 2.0% during 14 d for the same modified electrode，indicating that the stability of the modified electrode was good. The RSD of five different batches electrodes was 1.7%，suggesting that the reproducibility of this electrode was excellent. This method was used to detect the remaining concentration of forchlorfenuron in real kiwifruit samples with average recoveries ranging from 102.7% to 109.1%，which was basically in agreement with that of liquid chromatography mass spectrometry methods.
Keywords：forchlorfenuron；zero current potentiometry；β-cyclodextin；electropolymerization；supramolecular recognition
氣相色譜-串聯(lián)質(zhì)譜法測(cè)定花椒中106種農(nóng)藥殘留及膳食暴露風(fēng)險(xiǎn)評(píng)估
陳敏，尹全，鄧強(qiáng)，劉茜，張義蓉，楊曉鳳*
（四川省農(nóng)業(yè)科學(xué)院農(nóng)業(yè)質(zhì)量標(biāo)準(zhǔn)與檢測(cè)技術(shù)研究所，成都 610066）
摘要：建立了固相萃取結(jié)合氣相色譜-串聯(lián)質(zhì)譜（GC-MS/MS）測(cè)定花椒中106種農(nóng)藥殘留量的方法。采用多反應(yīng)監(jiān)測(cè)（MRM）模式檢測(cè)，基質(zhì)匹配標(biāo)準(zhǔn)曲線法定量。結(jié)果表明：106種農(nóng)藥的定量限（LOQ）范圍為0.010~0.10 mg/kg，且在定量限~1.0 mg/L范圍內(nèi)線性關(guān)系良好，線性相關(guān)系數(shù)R2≥0.99。106種農(nóng)藥的平均加標(biāo)回收率在60.8%~118.6%之間，相對(duì)標(biāo)準(zhǔn)偏差（RSD）在0.79%~19%之間。將該方法用于53批次市售花椒樣品的篩查，結(jié)果檢出21種農(nóng)藥殘留，其中有最大殘留限量值（MRL）的農(nóng)藥有9種，無(wú)MRL值的農(nóng)藥有12種。無(wú)MRL值的農(nóng)藥慢性膳食攝入風(fēng)險(xiǎn)值（ADI）為0.002%~0.343%，12種農(nóng)藥ADI總計(jì)為1.03%，花椒中農(nóng)藥殘留的膳食攝入風(fēng)險(xiǎn)較低。
關(guān)鍵詞：氣相色譜-串聯(lián)質(zhì)譜；花椒；固相萃取；農(nóng)藥多殘留；膳食風(fēng)險(xiǎn)評(píng)估
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）01-0070-09
Determination of 106 pesticide residues by gas chromatography-tandem mass spectrometry and dietary exposure risk assessment in Chinese prickly ash
CHEN Min，YIN Quan，DENG Qiang，LIU Qian，ZHANG Yirong，YANG Xiaofeng*
Institute of Quality and Testing Technology for Agro-products of Sichuan Academy of Agricultural Sciences，Chengdu 610066，China）
Abstract：A method for the determination of 106 pesticide residues in Chinese prickly ash by solid phase extraction （SPE） combined with gas chromatography-tandem mass spectrometry （GC-MS/MS）was developed. The samples were detected by multiple-reaction monitoring scanning and quantified using the matrix-matched standard calibration method. The results showed that the limits of quantification（LOQs） of 106 pesticides ranged from 0.010 to 0.10 mg/kg. There were good linear relationships in the range of LODs-1.0 mg/L，with the correlation coefficients R2≥0.99. The average recoveries for the 106 pesticides at three spiked levels were 60.8%- 118.6%，and the relative standard deviations （RSDs） were between 0.79% and 19%. The method was applied to the screening of 53 sample batches，the results showed that 21 pesticide residues were detected，including 9 kinds with maximum residue limits （MRLs） for pesticides and 12 kinds without MRLs. The chronic dietary intake risk （ADI） was 0.002%-0.343%，and the total ADI of 12 pesticides was 1.03%，so the dietary intake risk of pesticide residues in Chinese prickly ash was low.
Keywords：gas chromatography-tandem mass spectrometry；Chinese prickly ash；solid phase extraction；pesticide multi-residue；dietary intake risk assessment
銀納米粒子修飾半導(dǎo)體薄膜SERS基底的仿真研究
鮑士仟，李東明，馬成舉*，張躍斌，李咪，金嘉升，張垚，張貽歆，劉洺，劉芊震
（西安石油大學(xué)理學(xué)院，西安 710065）
摘要：設(shè)計(jì)了一種銀納米粒子（Ag NPs）修飾的半導(dǎo)體薄膜鍺（Ge）表面增強(qiáng)拉曼散射（SERS）基底。利用時(shí)域有限差分（FDTD）方法仿真分析了該SERS基底的消光光譜、局域電場(chǎng)和SERS特性，考察了Ag NPs半徑和Ge薄膜厚度對(duì)SERS基底拉曼散射信號(hào)增強(qiáng)的影響。對(duì)比分析了硅（Si）、砷化鎵（GaAs）、砷化銦（InAs）和Ge薄膜對(duì)SERS基底拉曼散射信號(hào)增強(qiáng)的影響。研究發(fā)現(xiàn)：Ag NPs半徑和半導(dǎo)體介電常數(shù)都會(huì)影響SERS基底拉曼散射信號(hào)的增強(qiáng)。通過(guò)計(jì)算發(fā)現(xiàn)，在半導(dǎo)體薄膜厚度為10 nm時(shí)，Ag NPs/Ge薄膜SERS基底在633 nm入射光激發(fā)下產(chǎn)生的增強(qiáng)因子（EF）高達(dá)7.02×107，對(duì)拉曼散射信號(hào)的增強(qiáng)作用最佳。
關(guān)鍵詞：銀納米粒子；半導(dǎo)體；時(shí)域有限差分法；局域電場(chǎng)；增強(qiáng)因子
中圖分類號(hào)：O433.4 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0079-07
Simulation study on semiconductor film SERS substrate modified by silver nanoparticles
BAO Shiqian，LI Dongming，MA Chengju*，ZHANG Yuebin，LI Mi，JIN Jiasheng，ZHANG Yao，ZHANG Yixin，LIU Ming，LIU Qianzhen
School of Science，Xi'an Shiyou University，Xi’an 710065，China）
Abstract：A kind of silver nanoparticles （Ag NPs） modified semiconductor germanium （Ge） film was designed as the surface-enhanced Raman scattering （SERS） substrates. The extinction spectra，local electric fields and SERS properties of the SERS substrates were simulated and analyzed by the finite difference time domain （FDTD） method. The influence of the radius of Ag NPs and the thickness of Ge film on the enhancement of Raman scattering signal of the SERS substrate was discussed. The influence of different film materials including silicon （Si），gallium arsenide （GaAs），indium arsenide （InAs），and Ge film on the enhancement of Raman scattering signal of the SERS substrate was further analyzed. It was found that both the radius of Ag NPs and the dielectric constant of semiconductor had effects on the enhancement of Raman scattering signal of the SERS substrate. It was found that when the semiconductor Ge film thickness was 10 nm，the SERS substrate of Ag NPs/Ge film under the excitation of 633 nm incident light had the high enhancement factor （EF） of 7.02×107，which provided the best enhancement effect on Raman scattering signal.
Keywords：silver nanoparticles；semiconductor；finite difference time domain method；local electric field；enhancement factor
基于金納米粒子探針比色法檢測(cè)乙基谷硫磷
張亞莉1，田璐肖2，徐鑫林1，王未肖1，哈婧*2
（1. 河北科技大學(xué)理學(xué)院，石家莊 050018；2. 河北科技大學(xué)化學(xué)與制藥工程學(xué)院，石家莊 050018）
摘要：基于乙基谷硫磷在酸性條件下可以誘導(dǎo)金納米粒子（AuNPs）發(fā)生聚集，建立了以AuNPs為探針、結(jié)合比色和分光光度法檢測(cè)乙基谷硫磷的方法。通過(guò)改變氯金酸和還原劑檸檬酸鈉的比例，制備了不同粒徑的AuNPs。酸性溶液中乙基谷硫磷分子中-P=S鍵發(fā)生質(zhì)子化，形成的-SH與Au形成S-Au鍵，使AuNPs發(fā)生聚集，溶液顏色由紅色轉(zhuǎn)變?yōu)樗{(lán)色。考察了乙酸-乙酸鈉緩沖溶液的pH和濃度以及乙基谷硫磷與AuNPs的作用時(shí)間對(duì)AuNPs聚集程度的影響。在優(yōu)化條件下，吸光度比值（A694 nm/A524 nm）與乙基谷硫磷濃度在0.392~0.603 μmol/L范圍內(nèi)具有良好的線性關(guān)系，檢出限為0.0782 μmol/L。
關(guān)鍵詞：金納米粒子；乙基谷硫磷；比色法；分光光度法；聚集
中圖分類號(hào)：TQ131；G642 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0086-05
Colorimetric detection of ethyazinphos-methyl based on gold nanoparticle probes
ZHANG Yali1，TIAN Luxiao2，XU Xinlin1，WANG Weixiao1，HA Jing*2
1. College of Sciences，Hebei University of Science and Technology，Shijiazhuang 050018，China；2. College of Chemical & Pharmacetical Engineering，Hebei University of Science and Technology，Shijiazhuang 050018，China）
Abstract：Based on the aggregation of gold nanoparticles （AuNPs） induced by ethyazinphos-methyl under acidic conditions，a new method for the detection of ethyazinphos-methyl using AuNPs as a probe combined with colorimetric and Uv-visible spectrophotometry was developed. AuNPs of different sizes were prepared by varying the ratio of sodium citrate to chloroauric acid. The -P=S bond was protonated in ethyl azinphos-methyl in acidic solution，the produced -SH formed an S-Au bond with Au，causing AuNPs aggregation and the color of the solution changed from red to blue. The effects of pH and concentration of acetic acid-sodium acetate buffer solution，and the interaction time between ethyazinphos-methyl and AuNPs were investigated. There was a good linear relationship between the absorbance ratio （A694 nm/A524 nm） and the concentration of ethyl azinphos-methyl in the range of 0.392-0.603 μmol/L，and the detection limit was 0.0782 μmol/L.
Keywords：gold nanoparticles；azinphos-ethyl；colorimetry；spectrophotometry；aggregate
基于ZIF-8電化學(xué)傳感器構(gòu)建及用于檢測(cè)飲料中新橙皮苷二氫查耳酮
張亮1，徐俊暉1，王亞珍*1，2
（1. 江漢大學(xué)光電材料與技術(shù)學(xué)院，武漢 430056；2. 湖北省健康代糖產(chǎn)品企校聯(lián)合創(chuàng)新中心，武漢 430056）
摘要：采用電泳沉積法，成功在玻碳電極（GCE）表面制備了一層ZIF-8材料薄膜，再在其表面滴涂一層全氟化樹脂溶液（Nafion），形成ZIF-8/Nafion復(fù)合膜，用于構(gòu)建檢測(cè)高倍甜味劑新橙皮苷二氫查耳酮（NHDC）的電化學(xué)傳感器。利用電化學(xué)交流阻抗（EIS）技術(shù)對(duì)該傳感器進(jìn)行表征，采用循環(huán)伏安法（CV）研究NHDC在ZIF-8/Nafion電極表面的電化學(xué)行為，并優(yōu)化實(shí)驗(yàn)條件。NHDC在ZIF-8/Nafion膜上有靈敏的響應(yīng)。采用差分脈沖伏安法（DPV）建立了定量檢測(cè)NHDC的方法，方法線性范圍為0.16~160 μmol/L，檢出限為56 nmol/L。該方法檢測(cè)飲料中NHDC的加標(biāo)回收率范圍為99.0%~101.3%。
關(guān)鍵詞：ZIF-8；電泳沉積法；新橙皮苷二氫查耳酮（NHDC）；電化學(xué)傳感器
中圖分類號(hào)：TS207.3；O657.1 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0091-07
Construction of ZIF-8 based electrochemical sensor for the detection of neohesperidin dihydrochalcone in beverage
ZHANG Liang1，XU Junhui1，WANG Yazhen*1，2
1. School of Optoelectronic Materials and Technology，Jianghan University，Wuhan 430056，China；2. Hubei Enterprise-College Joint Innovation Center of Healthy Sugar Substitute Product，Wuhan 430056，China）
Abstract：The electrophoretic deposition method was used to prepare ZIF-8 film on the surface of glassy carbon electrode （GCE），then an amount of perfluorinated resin solution （Nafion） was dropped on the surface of ZIF-8 modified GCE，and thus a ZIF-8/Nafion composite film modified electrode（ZIF-8/Nafion GCE） was obtained and an electrochemical sensor for the high concentration of sweetener neohesperidin dihydrochalcone （NHDC） was constructed. The sensor was electrochemically characterized by electrochemical impedance spectroscopy （EIS），the electrochemical behavior of NHDC on the surface of the ZIF-8/Nafion GCE electrode was investigated，and the experimental conditions were optimized by using the cyclic voltammetry （CV） method. The sensor evinced a sensitive response to NHDC on the ZIF-8/Nafion GCE electrode. Differential pulse voltammetry （DPV） method was used to establish a quantitative detection method for NHDC with a linear range of 0.16-160 μmol/L and a detection limit of 56 nmol/L. The spiked recoveries of this method for the detection of NHDC in beverages were 99.0%-101.3%.
Keywords：ZIF-8；electrophoretic deposition；neohesperidin dihydrochalcone （NHDC）；electrochemical sensor
八面體二氧化鈰負(fù)載金納米粒子的電化學(xué)傳感器檢測(cè)鄰氨基苯酚
黃青1，諸葛文鳳1，凌晨東2，張翠忠1，向剛1，彭金云*1，黃海冰1
（1. 廣西民族師范學(xué)院化學(xué)與生物工程學(xué)院，光電化學(xué)傳感與區(qū)域環(huán)境分析實(shí)驗(yàn)室，崇左 532200；2. 中國(guó)-泰國(guó)崇左產(chǎn)業(yè)園管理委員會(huì)，崇左 532200）
摘要：采用原位生長(zhǎng)法制備了八面體二氧化鈰（CeO2）負(fù)載金納米粒子（Au NPs）復(fù)合材料Au NPs@ CeO2，用掃描電鏡及能量色散X射線光譜儀對(duì)復(fù)合材料進(jìn)行形貌表征與元素分析。利用此復(fù)合材料修飾玻碳電極，構(gòu)筑了一種鄰氨基苯酚電化學(xué)傳感器。CeO2性質(zhì)穩(wěn)定，其八面體結(jié)構(gòu)提供了較大的比表面積，Au NPs具備極佳的導(dǎo)電性，二者復(fù)合協(xié)同發(fā)揮良好的電催化能力。研究發(fā)現(xiàn)，Au NPs@CeO2復(fù)合材料修飾電極對(duì)鄰氨基苯酚表現(xiàn)出較高的檢測(cè)靈敏度，在優(yōu)化實(shí)驗(yàn)條件下，鄰氨基苯酚濃度與氧化峰電流成正比，在1.00×10-7~3.38×10-5 mol/L濃度范圍內(nèi)呈現(xiàn)2段較好的線性關(guān)系，線性回歸方程分別為I1（A）=3.29×10-2c（mol/L）+1.08×10-8 （R=0.9967）和I2（A）=1.32×10-2c（mol/L）+1.22×10-7 （R=0.9956），檢出限（LOD）為1.16×10-8 mol/L。該電化學(xué)傳感器用于實(shí)際樣品中鄰氨基苯酚的測(cè)定，回收率為98.0%~105.3%，相對(duì)標(biāo)準(zhǔn)偏差為0.9%~3.1%。
關(guān)鍵詞：二氧化鈰；金納米粒子；電化學(xué)傳感器；鄰氨基苯酚
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）01-0098-06
An electrochemical sensor based on the octahedral cerium dioxide-loaded gold nanoparticles for the detection of o-aminophenol
HUANG Qing1，ZHUGE Wenfeng1，LING Chendong2，ZHANG Cuizhong1，XIANG Gang1，PENG Jinyun*1，HUANG Haibing1
1. Photochemical Sensing and Regional Environmental Analysis Laboratory，Chemical and Biological Engineering College，Guangxi Normal University for Nationalities，Chongzuo 532200，China；2. China- Thailand Chongzuo Industrial Park Management Committee，Chongzuo 532200，China）
Abstract：The composite of octahedral cerium dioxide-loaded gold nanoparticles （Au NPs@CeO2） was prepared by the in-situ growth method. The morphology and elemental analysis of the composite were characterized by scanning electron microscope and energy dispersion X-ray spectrometer. An o-amino phenol electrochemical sensor was constructed by using the composite modified glass carbon electrode. The octahedral cerium dioxide （CeO2） has the advantages of stable chemical property and a large specific surface area. It has excellent electrocatalytic performance in combination with gold nanoparticles （Au NPs）. It was found that Au NPs@CeO2 modified electrode showed high detection sensitivity to o-aminophenol. Under the optimal experimental conditions，the concentration of o-aminophenol was proportional to the oxidation peak current，and there were two good linear relationships between the concentration of o-aminophenol and the oxidation peak current in the range of 1.00×10-7-3.38×10-5 mol/L. The linear regression equations were I1（A）=3.29×10-2c（mol/L）+1.08×10-8 （R=0.9967） and I2（A）=1.32×10-2c（mol/L）+1.22×10-7 （R=0.9956），respectively. The detection limit （LOD） was 1.16×10-8 mol/L. The electrochemical sensor could be used for rapid detection of o-aminophenol in real samples，the recoveries of o-aminophenol were 98.0%-105.3%，and the relative standard deviations were 0.9%-3.1%.
Keywords：cerium dioxide；gold nanoparticles；electrochemical sensor；o-aminophenol
基于低共熔溶劑的分散液液微萃取-高效液相色譜法測(cè)定環(huán)境水樣和飲料中的柯依定、金胺O和羅丹明B
于洋，曹天薈，羅安夢(mèng)，高樹林*，葛丹丹
（昆明學(xué)院化學(xué)化工學(xué)院，昆明 650214）
摘要：建立了基于低共熔溶劑的渦旋輔助分散液液微萃取-高效液相色譜聯(lián)用檢測(cè)柯衣定、金胺O和羅丹明B的方法。以香芹酚為氫鍵給體，薄荷醇、正癸酸或正辛酸為氫鍵受體，制備疏水性低共熔溶劑（DESs）并作為萃取溶劑。采用紅外光譜（FT-IR）和量子化學(xué)計(jì)算研究DESs的形成機(jī)理。對(duì)DESs組成、萃取溶劑體積、萃取時(shí)間、溶液pH和鹽濃度等實(shí)驗(yàn)條件進(jìn)行了優(yōu)化。在最優(yōu)化條件下，柯衣定、金胺O和羅丹明B在5~1000 ng/mL范圍內(nèi)線性關(guān)系良好，相關(guān)系數(shù)均大于0.9950，檢出限和定量限分別為1.0~1.5 ng/mL和3.5~4.7 ng/mL。模擬計(jì)算研究表明，DESs萃取3種合成色素的主要作用力是氫鍵和靜電相互作用力。將所建立的方法用于檢測(cè)環(huán)境水樣和飲料樣品中的金胺O、羅丹明B和柯衣定，加標(biāo)回收率為85.7%~106.8%，相對(duì)標(biāo)準(zhǔn)偏差為0.2%~7.7%。
關(guān)鍵詞：疏水性低共熔溶劑；模擬計(jì)算；合成色素；分散液-液微萃取；高效液相色譜法
中圖分類號(hào)：O661.1 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0104-07
Determination of chrysoidin，auramine O and rhodamine B in environmental water and beverage by deep eutectic solvents based dispersive liquid-liquid microextraction combined with high performance liquid chromatography
YU Yang，CAO Tianhui，LUO Anmeng，GAO Shulin*，GE Dandan
School of Chemistry and Chemical Engineering，Kunming University，Kunming 650214，China）
Abstract：A vortex-assisted liquid-liquid microextraction method combined with high performance liquid chromatography-diode array detector was established for the determination of chrysoidin，auramine O and rhodamine B in environmental water and beverage. The water-immiscible deep eutectic solvents （DESs） were prepared using carvacrol as hydrogen-bonding donor and menthol，n-decanoic acid or n-octanoic acid as hydrogen-bonding acceptor at different molar ratios，and the DESs were used as extraction solvents. The formation mechanism of DESs was investigated using Fourier transform infrared spectroscopy （FT-IR） and quantum chemical calculations. Several parameters influencing the extraction efficiencies of synthetic dyes including types of DESs，volume of extraction solvent，extraction time，pH of solution and salt concentration were optimized. Under the optimum conditions，synthetic dyes can be determined in the range of 5.0-1000 ng/mL with the coefficient higher than 0.9950. Limits of detection of the method ranged from 1 to 1.5 ng/mL and limits of quantification were in a range of 3.5-4.7 ng/mL. The possible interactions of DESs with synthetic dyes were investigated by computational modeling. The results revealed that hydrogen bonds and electrostatic interactions were the main driving forces for the extraction of synthetic dyes. The proposed method was applied to determine the synthetic dyes in environmental water and beverage with the recoveries in the range of 85.7%-106.8% and the relative standard deviations （RSDs） between 0.2%-7.7%.
Keywords：hydrophobic deep eutectic solvents；computational modeling；synthetic dyes；dispersive liquid-liquid microextraction；high performance liquid chromatography
用于磁珠法核酸提取的微流控芯片及自動(dòng)化平臺(tái)
劉晨曦，姚延祿，周新麗*
（上海理工大學(xué)健康科學(xué)與工程學(xué)院，上海 200093）
摘要：基于磁珠法核酸提取原理，設(shè)計(jì)并制作出旋轉(zhuǎn)驅(qū)動(dòng)式核酸提取微流控芯片及自動(dòng)化平臺(tái)。微流控芯片包括裂解腔、清洗腔以及洗脫腔等結(jié)構(gòu)，步進(jìn)電機(jī)帶動(dòng)微流控芯片旋轉(zhuǎn)，通過(guò)電磁鐵吸附微流控芯片內(nèi)的磁珠，實(shí)現(xiàn)磁珠在各腔室轉(zhuǎn)移，完成核酸提取和純化。對(duì)芯片表面疏水性、磁力大小、磁珠分散程度以及核酸洗脫時(shí)間進(jìn)行優(yōu)化。結(jié)果表明，當(dāng)磁力大小為250 N時(shí)，可實(shí)現(xiàn)磁珠轉(zhuǎn)移；磁鐵放置于芯片上方1 mm時(shí)，腔室內(nèi)磁珠分散程度最好。洗脫時(shí)間為20 min時(shí)，芯片上提取大腸桿菌的核酸濃度較高。微流控芯片與磁珠核酸提取技術(shù)相結(jié)合提取的核酸樣本，可直接應(yīng)用于后續(xù)聚合酶鏈?zhǔn)椒磻?yīng)擴(kuò)增環(huán)節(jié)，有利于實(shí)現(xiàn)核酸自動(dòng)提取及擴(kuò)增的一體化。
關(guān)鍵詞：微流控技術(shù)；核酸提取；磁珠法；自動(dòng)化提取
中圖分類號(hào)：R331 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0111-07
Microfluidic chip and automation platform for nucleic acid extraction by magnetic bead method
LIU Chenxi，YAO Yanlu，ZHOU Xinli*
School of Health Science and Engineering，University of Shanghai for Science and Technology，Shanghai 200093，China）
Abstract：Based on the principle of magnetic bead method for nucleic acid extraction，a rotary-driven microfluidic chip and an automation platform were designed and manufactured. The microfluidic chip includes a lysis chamber，a cleaning chamber and an elution chamber. The stepping motor drives the microfluidic chip to rotate. The magnetic beads in the microfluidic chip are adsorbed by the electromagnet to realize the transfer of the magnetic beads between each chamber. In this way，nucleic acid extraction and purification are completed. The hydrophobicity of the chip surface，the magnitude of the magnetic force，the degree of magnetic beads dispersion，and the elution time of nucleic acid were optimized，respectively. The results showed that when the magnetic force was 250 N，the transfer of magnetic beads were capable of realizing. When the magnet was placed 1 mm above the chip，the magnetic beads in the chamber was well dispersed. When the elution time was 20 min，the nucleic acid concentration of E. coli extracted on the chip was higher. The nucleic acid samples extracted by the microfluidic chip cooperating with magnetic bead nucleic acid extraction technology can be directly applied to the subsequent polymerase chain reaction amplification. This is beneficial to realize the integration of nucleic acid automatic extraction and amplification.
Keywords：microfluidics；nucleic acid extraction；magnetic bead method；automated extraction
分子印跡聚合物在核苷類藥物分離分析中的應(yīng)用
薛俊萍，魏國(guó)，柴佩君，吳文璞，張異夢(mèng)，李桂生*，宋志花*
（新型制劑與生物技術(shù)藥物研究山東省高校協(xié)同創(chuàng)新中心，分子藥理和藥物評(píng)價(jià)教育部重點(diǎn)實(shí)驗(yàn)室，煙臺(tái)大學(xué)藥學(xué)院，煙臺(tái) 264005）
摘要：核苷類藥物在新型冠狀病毒肺炎（COVID-19）、艾滋病及肝炎等病毒性疾病治療方面效果顯著，應(yīng)用廣泛，其準(zhǔn)確定量具有重要意義。近年來(lái)，基于分子印跡技術(shù)合成的分子印跡聚合物（MIPs）備受關(guān)注。MIPs可模擬酶與底物或抗體與抗原之間的相互作用，對(duì)目標(biāo)物進(jìn)行高選擇性識(shí)別。將MIPs應(yīng)用于核苷類藥物分離分析過(guò)程，可顯著提高選擇性和檢測(cè)靈敏度。本文對(duì)近5年MIPs在核苷類藥物樣品前處理（固相萃取、固相微萃取等）、色譜分離及傳感分析等檢測(cè)中的應(yīng)用進(jìn)行綜述，總結(jié)了檢測(cè)過(guò)程中面臨的挑戰(zhàn)，并對(duì)其應(yīng)用前景進(jìn)行了展望。
關(guān)鍵詞：分子印跡聚合物；核苷類藥物；樣品前處理；色譜分析；傳感分析
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）01-0118-10
Applications of molecularly imprinted polymers in separation and analysis of nucleoside drugs
XUE Junping，WEI Guo，CHAI Peijun，WU Wenpu，ZHANG Yimeng，LI Guisheng*，SONG Zhihua*
Ministry of Education，Collaborative Innovation Center of Advanced Drug Delivery System and Biotech Drugs in Universities of Shandong，Key Laboratory of Molecular Pharmacology and Drug Evaluation，School of Pharmacy，Yantai University，Yantai 264005，China）
Abstract：Nucleoside drugs are effective in the treatment of novel coronavirus pneumonia （COVID-19），HIV，hepatitis and other viral diseases in recent years. Therefore，the accurate quantitative analysis of them is of great significance. For the past few years，molecularly imprinted polymers （MIPs） synthesized by molecular imprinting technology have attractedmuch attention. The MIPs can stimulate the interactions between enzymes with substrates or antibodies and antigens，and support a recognition of the target with high selectivity. The selectivity and sensitivity can be greatly improved using MIPs in the separation and analysis of nucleoside drugs. In this review，the applications of MIPs in three fields including sample pretreatment （solid phase extraction，solid phase microextraction，etc.），chromatographic separation and sensor analysis of nucleoside drugs in the last five years are summarized. The advantages of MIPs in detection of nucleoside drugs are discussed. Meanwhile，the challenges and prospects are expected.
Keywords：molecularly imprinted polymers （MIPs）；nucleoside drugs；sample pretreatment；chromatographic analysis；sensor analysis
基于智能手機(jī)現(xiàn)場(chǎng)快速檢測(cè)技術(shù)研究進(jìn)展
唐博1，陳佳敏1，韓永輝*1，2，崔建升*1，劉大喜1
（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. 河北省固體廢棄物資源化技術(shù)創(chuàng)新中心，石家莊 050018）
摘要：作為一種便攜式的功能性移動(dòng)電子設(shè)備，智能手機(jī)的廣泛應(yīng)用為便攜式檢測(cè)提供了發(fā)展平臺(tái)，并在臨床診斷、食品安全分析和環(huán)境監(jiān)測(cè)等領(lǐng)域表現(xiàn)出巨大的應(yīng)用潛力。本文綜述了2018~2022年，基于智能手機(jī)與比色法、熒光法、化學(xué)發(fā)光法、電化學(xué)分析、免疫分析及微流控分析等技術(shù)聯(lián)用的即時(shí)檢測(cè)應(yīng)用研究進(jìn)展，并對(duì)其發(fā)展趨勢(shì)和應(yīng)用前景進(jìn)行了展望。
關(guān)鍵詞：智能手機(jī)；即時(shí)檢測(cè)；綜述
中圖分類號(hào)：O657 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0128-11
Advances in portable detection technology based on smartphone
TANG Bo1，CHEN Jiamin1，HAN Yonghui*1，2，CUI Jiansheng*1，LIU Daxi1
1. College of Environmental Science and Engineering，Hebei University of Science and Technology，Shijiazhuang 050018，China；2. Hebei Technology Innovation Centre of Solid Wastes Utilization，Shijiazhuang 050018，China）
Abstract：As a portable functional mobile electronic device，the wide application of smartphones provides a tremendous platform for the development of portable detection，which shows great potential for application in the fields of clinical diagnosis，food safety analysis，and environmental monitoring. In this review，the advances in real-time detection application based on smart phone combined with colorimetry，fluorescence，chemiluminescence，electrochemical analysis，immunoassay and microfluidic analysis from 2018 to 2022 were summaried，and provides a prospect of the development trend of this technology in analytical testing.
Keywords：smartphone；point-of-care testing；review
藥食同源中藥材鑒定技術(shù)研究進(jìn)展
謝以清1，2，符鴿3，閏凌君1，閆萌萌1，2，雷海民2，馬強(qiáng)*1
（1. 中國(guó)檢驗(yàn)檢疫科學(xué)研究院，北京 100176；2. 北京中醫(yī)藥大學(xué)中藥學(xué)院，北京102488；3. 中國(guó)消費(fèi)品質(zhì)量安全促進(jìn)會(huì)，北京 100125）
摘要：藥食同源中藥材具有營(yíng)養(yǎng)和藥用的雙重價(jià)值，因此被廣泛應(yīng)用于食品、醫(yī)藥等領(lǐng)域。藥食同源中藥材鑒定是藥食同源中藥材應(yīng)用的基礎(chǔ)。近年來(lái)，隨著各學(xué)科內(nèi)容和方法的豐富和創(chuàng)新，藥食同源中藥材鑒定技術(shù)也得到了發(fā)展，涌現(xiàn)出一些新的技術(shù)和方法。同時(shí)，多元化的現(xiàn)代鑒定技術(shù)和傳統(tǒng)鑒定技術(shù)形成了相互補(bǔ)充、相互促進(jìn)的關(guān)系，有利于研究制定規(guī)范化的藥食同源中藥材質(zhì)量標(biāo)準(zhǔn)，并推動(dòng)中醫(yī)藥的現(xiàn)代化、科學(xué)化、國(guó)際化創(chuàng)新發(fā)展。本文介紹了藥食同源中藥材的歷史背景和發(fā)展現(xiàn)狀，總結(jié)了傳統(tǒng)經(jīng)驗(yàn)鑒定、分子生物學(xué)鑒定、光譜鑒定、色譜-質(zhì)譜聯(lián)用鑒定等各種鑒定技術(shù)的特點(diǎn)和優(yōu)勢(shì)，對(duì)國(guó)內(nèi)外新技術(shù)、新方法的應(yīng)用進(jìn)行了重點(diǎn)闡述，并對(duì)藥食同源中藥材鑒定技術(shù)的發(fā)展趨勢(shì)進(jìn)行了展望，以期為相關(guān)領(lǐng)域技術(shù)人員提供參考。
關(guān)鍵詞：藥食同源中藥材；鑒定技術(shù)；研究進(jìn)展
中圖分類號(hào)：R282.5 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：1000-0720（2024）01-0139-10
Research progress of identification techniques on medicinal and edible traditional Chinese medicine
XIE Yiqing1，2，F(xiàn)U Ge3，RUN Lingjun1，YAN Mengmeng1，2，LEI Haimin2，MA Qiang*1
1. Chinese Academy of Inspection and Quarantine，Beijing 100176，China；2. School of Chinese Materia Medica，Beijing University of Chinese Medicine，Beijing 102488，China；3. China Association for Consumer Products Quality and Safety Promotion，Beijing 100125，China）
Abstract：Medicinal and edible traditional Chinese medicine has both nutritional and medicinal values，and therefore is widely used in the fields of food and medicine. The identification techniques of medicinal and edible traditional Chinese medicine are the basis of its applications. In recent years，with the enrichment and innovation of the contents and methods of various subjects，the identification technologies of Chinese herbal medicines with homology of medicine and food have also been developed，and some new technologies and methods have emerged. Moreover，diversified modern and traditional identification techniques are mutually complementing and promoting，which are beneficial for the formulation of quality standards as well as the modernization，scientification，and internationalization of medicinal and edible traditional Chinese medicine. In this paper，the historical background and current development of medicinal and edible traditional Chinese medicine were introduced. The characteristics and advantages of various identification techniques，such as identification based on traditional experience，molecular biology，spectroscopy，and hyphenation of chromatography and mass spectrometry were summarized. The applications of novel techniques and methods were highlighted. The future prospect of the identification techniques of medicinal and edible traditional Chinese medicine was discussed. This paper may provide a useful guidance for relevant researchers in this field.
Keywords：medicinal and edible traditional Chinese medicine；identification techniques；research progress
