《分析試驗室》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磺胺甲噁唑
武天恒，劉蕊*，韓雪，劉日嘉，孫源
（哈爾濱商業大學藥學院藥物工程技術研究中心，哈爾濱 150076）
摘要：通過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BiOI/g-C3N4納米復合材料的微觀結構和形貌進行了表征。通過滴涂法將BiOI/g-C3N4復合材料修飾在玻碳電極（GCE）表面，構建了用于快速檢測磺胺甲噁唑（SMX）的電化學傳感平臺，通過循環伏安（CV）和差分脈沖伏安（DPV）技術對SMX進行電化學分析，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。采用加標回收法測定自來水樣品中的SMX，加標回收率為90.0%~103.4%。
關鍵詞：g-C3N4納米片；電化學傳感器；磺胺甲噁唑
中圖分類號：O657.1；X703 文獻標識碼：A 文章編號：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分析平臺在胃癌早期診斷中的應用研究
韋偉1，朱群山3，黃永1，石立新6，吳正3，楊永國4，劉佳2，袁夢軒5，王震光1，蔣豐娟*2
（1. 揚州大學附屬江都人民醫院胃腸外科，揚州 225200；2. 揚州大學附屬江都人民醫院消化內科，揚州 225200；3. 揚州大學附屬江都人民醫院普通外科，揚州 225200；4. 揚州大學附屬江都人民醫院病理科，揚州 225200；5. 揚州大學附屬江都人民醫院放射科，揚州225200；6. 揚州大學附屬江都人民醫院檢驗科，揚州 225200）
摘要：利用界面自組裝方法制備了具有優良均一性、穩定性和SERS活性的金銀納米梭（Au-AgNSs）基底。通過將4-巰基苯甲酸（4-MBA）修飾在Au-AgNSs基底表面，并結合癌胚抗原（CEA）的單克隆抗體，實現了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發生形變，導致特征峰發生偏移。經驗證，該基于拉曼頻移的SERS分析平臺具有優異的特異性、重復性和靈敏度，對血清中CEA的檢測限（LOD）低至1.22 pg/mL。利用其對胃癌（GC）患者和健康受試者血清中CEA的表達水平進行測定，并與酶聯免疫吸附測定法（ELISA）結果比較。結果表明，GC患者血清CEA表達水平高于健康受試者，且2種方法結果無明顯差異。因此基于拉曼頻移的SERS分析平臺在GC診斷中具有應用價值。
關鍵詞：拉曼頻移；表面增強拉曼散射；胃癌；早期診斷；生物標志物
中圖分類號：O657.37 文獻標識碼：A 文章編號：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
構建電化學適配體傳感器快速檢測中藥材中的赭曲霉毒素A
范申，黃榕芬，毛偉偉，張紅艷*
（福建中醫藥大學藥學院，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復合材料，制備修飾電極，結合赭曲霉毒素A（OTA）的特異性適配體，構建高靈敏度電化學生物傳感器，并用于中藥中OTA的含量測定。在最優條件下，峰電流變化值與OTA濃度對數值的線性響應范圍為2.3 pmol/L~2.3 nmol/L，檢測限為0.53 pmol/L。應用該方法對中藥飲片中OTA的含量進行加標回收實驗，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。
關鍵詞：赭曲霉毒素A；電化學適配體傳感；快速檢測；中藥材
中圖分類號：O657.1 文獻標識碼：A 文章編號：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，Fuzhou 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. 山西中醫藥大學中藥與食品工程學院，晉中 030619；2. 桂林醫學院藥學院，桂林 541004）
摘要：構建了一種基于羧基化單壁碳納米角 （oxSWCNHs）的簡單、靈敏的熒光傳感體系用于胰蛋白酶的檢測。實驗中合成了水溶性的oxSWCNHs，并設計了一段羧基熒光素（FAM）標記肽段作為胰蛋白酶的底物，該底物能與胰蛋白酶進行特異性反應。當體系中沒有胰蛋白酶存在時，FAM標記的肽段可以被oxSWCNHs強烈吸附，致使體系具有較低的熒光背景；當體系中有胰蛋白酶存在時，胰蛋白酶可以與其底物肽段發生特異性水解反應，導致FAM標記的肽段水解為單個氨基酸，致使FAM遠離oxSWCNHs表面，FAM熒光不能被oxSWCNHs淬滅，體系具有較強的熒光強度，從而實現熒光傳感體系對胰蛋白酶的檢測。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定。
關鍵詞：單壁碳納米角；熒光傳感體系；胰蛋白酶
中圖分類號：O657.39 文獻標識碼：A 文章編號：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，FAM-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
基于量子點微球免疫層析法快速靈敏檢測雞肉中甲氧芐啶
謝敏1，費丹1，徐俊1，賴科洋2，陳媛3，羅凱3，彭娟4，周瑤敏*1
（1. 農業農村部禽類產品質量安全控制重點實驗室，江西省農業科學院農產品質量安全與標準研究所，南昌 330200；2. 荷蘭瓦赫寧根大學及研究中心，瓦赫寧根 6700AA；3. 江西維邦生物科技有限公司，南昌 330029；4. 南昌大學食品科學與技術國家重點實驗室，南昌 330047）
摘要：建立了一種快速靈敏檢測甲氧芐啶的量子點微球免疫層析法，對pH、標記抗體濃度、試紙條檢測線上的抗原濃度以及試紙條結合墊上的探針體積進行了優化。通過量子點微球試紙條檢測儀讀取試紙條上檢測線和質控線的熒光信號強度，以甲氧芐啶的濃度為橫坐標，檢測線和質控線熒光信號強度的比值為縱坐標，建立標準曲線。結果表明，方法定量檢測范圍為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%的交叉反應率。該方法適合大批量樣品的現場篩查。
關鍵詞：量子點微球；甲氧芐啶；檢測；免疫層析法
中圖分類號：O657.6 文獻標識碼：A 文章編號：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，FEI 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比色法特異性檢測廢水中新冠病毒靶標RNA
張琳，張穎，宋九華，韓耀霞，楊孝容，雷欣夢，黃莉翔，徐君茹，何思儀，邱小鳳，史鎧*
（樂山師范學院新能源材料與化學學院，樂山 614000）
摘要：基于Toehold介導的鏈置換反應（TSDR）與DNA酶，構建了一個強特異性及低成本檢測廢水中SARS-CoV-2靶標RNA單堿基突變的比色生物傳感器。SARS-CoV-2靶標RNA與雙鏈DNA（dsDNA）引發TSDR，釋放出完整的G-四鏈體序列并與氯化血紅素（Hemin）結合，形成G-四鏈體/Hemin DNA酶，進而催化雙氧水氧化3，3’，5，5’-四甲基聯苯胺，使溶液呈藍色。當SARS-CoV-2靶標RNA存在單堿基突變時，TSDR被抑制，導致裸眼觀察到的溶液顏色與未突變異的靶標相比更淺。同時采用智能手機攝像頭捕捉溶液的RGB值變化（ΔRGB），對裸眼觀察結果的準確性進行驗證。在最優條件下，構建的比色生物傳感器能夠特異性識別單個堿基突變的SARS-CoV-2靶標RNA，具有用于廢水中SARS-CoV-2變異毒株檢測的潛力。
關鍵詞：新冠病毒靶標RNA；Toehold鏈置換；智能手機；廢水
中圖分類號：O654.2 文獻標識碼：A 文章編號：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3
（1. 吉林農業大學資源與環境學院，長春 130118；2. 秸稈綜合利用與黑土保護教育部重點實驗室，吉林農業大學生命科學學院，長春 130118；3. 赤峰學院化學化工學院，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，模擬優化DES 和MAA作用的摩爾比例，并考察了DES印跡作用的機理。通過靜態吸附、動態吸附、選擇吸附、競爭吸附方法考察了DES-MIPs的親和性與選擇性。結果表明：DES與MAA之間通過氫鍵相互作用，當DES與MAA摩爾比為1∶5時，形成DES-MAA有序排列的復合物氫鍵數目最多（9），結合能最低（-146.62 kJ/mol）。該條件下制備的DES-MIPs對DES的最大吸附量為60.17 mg/g，且其動力學吸附符合準二級動力學模型。在一元及二元吸附體系中，DES-MIPs對DES都具有優異的選擇吸附性。
關鍵詞：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：O641.3 文獻標識碼：A 文章編號：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-串聯質譜法測定化妝品中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. 湖南省藥品檢驗檢測研究院，湖南省藥品質量評價工程技術研究中心，長沙 410001；2. 山東省食品藥品檢驗研究院，濟南 250101）
摘要：建立并驗證了超高效液相色譜-串聯質譜法（UHPLC-MS）同時測定化妝品中他克莫司、吡美莫司、依維莫司、西羅莫司、環孢菌素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相，多反應監測模式下測定，外標法定量。結果表明，這5種免疫抑制劑在0.5~100 ng/mL濃度范圍內線性關系良好，方法檢出限均低于10 ng/g，在不同化妝品基質中低、中、高3個濃度水平的加標回收率為93.3%~117.4%，相對標準偏差（RSD）為0.4%~7.5%。日內RSD為2.4%~8.4%，日間RSD為3.9%~26%。該方法彌補了化妝品中非法添加違禁物質檢測方法的缺失，為化妝品日常監管提供技術支撐。
關鍵詞：免疫抑制劑；化妝品；超高效液相色譜-串聯質譜
中圖分類號：TQ658.2 文獻標識碼：A 文章編號：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譜裂解規律研究
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研究重點實驗室，浙江警察學院，杭州 310053；2. 浙江省禁毒和毒情監測關鍵技術研究重點實驗室，國家毒品實驗室浙江分中心，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）電離模式下的質譜裂解規律，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-質譜聯用（GC-MS）和液相色譜-高分辨質譜聯用（LC-Q-Orbitrap/MS）技術，對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程進行分析，并對獲得的質譜圖進行解析，推測該類合成大麻素的EI-MS及ESI-MSn碎裂規律。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構推斷。碎片離子6，7和8對應的質荷比（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+），以及通過腙鍵及N1與側鏈之間發生斷裂（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末端取代側鏈。本研究闡述了5種新型靛紅腙類合成大麻素的質譜裂解規律，并根據獲得的質譜裂解規律建立了可疑物中該類合成大麻素的鑒定方法，為其快速結構鑒定提供依據。
關鍵詞：靛紅腙類合成大麻素；質譜裂解規律；快速篩查；電子轟擊質譜；電噴霧質譜
中圖分類號：O657.31；X832 文獻標識碼：A 文章編號：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-環糊精修飾電極零流電位法檢測氯吡脲
馬明明*1，何成毅2，史帥1，崔淑慧1，劉佳1
（1. 西安工程大學環境與化學工程學院，西安 710048；2. 西安市農產品質量安全檢驗監測中心，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-環糊精-氯吡脲（CPPU）復合材料（P-β-CD-CPPU），并對其結構和形貌進行表征。結果表明，含有CPPU分子殘留活性點的P-β-CD-CPPU擁有較大筒腔結構，能重新包合識別CPPU分子，據此建立了P-β-CD-CPPU修飾電極零流電位法檢測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范圍內成正比，CPPU的檢出限為21.4 nmol/L。CPPU體系可能共存的有機物及金屬離子均不干擾測定；同一根修飾電極對同一濃度CPPU零流電位測定值在14 d內的相對標準偏差（RSD）為2.0%；5根不同批次修飾電極的零流電位測定值的RSD為1.7%。應用本方法檢測實際獼猴桃樣品中CPPU殘留濃度，平均回收率為102.7%~109.1%，與液相色譜-質譜聯用法檢測結果基本一致。
關鍵詞：氯吡脲；零流電位法；β-環糊精；電聚合；超分子識別
中圖分類號：O657.1；O625.63 文獻標識碼：A 文章編號：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-串聯質譜法測定花椒中106種農藥殘留及膳食暴露風險評估
陳敏，尹全，鄧強，劉茜，張義蓉，楊曉鳳*
（四川省農業科學院農業質量標準與檢測技術研究所，成都 610066）
摘要：建立了固相萃取結合氣相色譜-串聯質譜（GC-MS/MS）測定花椒中106種農藥殘留量的方法。采用多反應監測（MRM）模式檢測，基質匹配標準曲線法定量。結果表明：106種農藥的定量限（LOQ）范圍為0.010~0.10 mg/kg，且在定量限~1.0 mg/L范圍內線性關系良好，線性相關系數R2≥0.99。106種農藥的平均加標回收率在60.8%~118.6%之間，相對標準偏差（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，結果檢出21種農藥殘留，其中有最大殘留限量值（MRL）的農藥有9種，無MRL值的農藥有12種。無MRL值的農藥慢性膳食攝入風險值（ADI）為0.002%~0.343%，12種農藥ADI總計為1.03%，花椒中農藥殘留的膳食攝入風險較低。
關鍵詞：氣相色譜-串聯質譜；花椒；固相萃?。晦r藥多殘留；膳食風險評估
中圖分類號：TS207.5；O657.63 文獻標識碼：A 文章編號：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
（西安石油大學理學院，西安 710065）
摘要：設計了一種銀納米粒子（Ag NPs）修飾的半導體薄膜鍺（Ge）表面增強拉曼散射（SERS）基底。利用時域有限差分（FDTD）方法仿真分析了該SERS基底的消光光譜、局域電場和SERS特性，考察了Ag NPs半徑和Ge薄膜厚度對SERS基底拉曼散射信號增強的影響。對比分析了硅（Si）、砷化鎵（GaAs）、砷化銦（InAs）和Ge薄膜對SERS基底拉曼散射信號增強的影響。研究發現：Ag NPs半徑和半導體介電常數都會影響SERS基底拉曼散射信號的增強。通過計算發現，在半導體薄膜厚度為10 nm時，Ag NPs/Ge薄膜SERS基底在633 nm入射光激發下產生的增強因子（EF）高達7.02×107，對拉曼散射信號的增強作用最佳。
關鍵詞：銀納米粒子；半導體；時域有限差分法；局域電場；增強因子
中圖分類號：O433.4 文獻標識碼：A 文章編號：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. 河北科技大學理學院，石家莊 050018；2. 河北科技大學化學與制藥工程學院，石家莊 050018）
摘要：基于乙基谷硫磷在酸性條件下可以誘導金納米粒子（AuNPs）發生聚集，建立了以AuNPs為探針、結合比色和分光光度法檢測乙基谷硫磷的方法。通過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鍵發生質子化，形成的-SH與Au形成S-Au鍵，使AuNPs發生聚集，溶液顏色由紅色轉變為藍色?？疾炝艘宜?乙酸鈉緩沖溶液的pH和濃度以及乙基谷硫磷與AuNPs的作用時間對AuNPs聚集程度的影響。在優化條件下，吸光度比值（A694 nm/A524 nm）與乙基谷硫磷濃度在0.392~0.603 μmol/L范圍內具有良好的線性關系，檢出限為0.0782 μmol/L。
關鍵詞：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：TQ131；G642 文獻標識碼：A 文章編號：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電化學傳感器構建及用于檢測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. 江漢大學光電材料與技術學院，武漢 430056；2. 湖北省健康代糖產品企校聯合創新中心，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復合膜，用于構建檢測高倍甜味劑新橙皮苷二氫查耳酮（NHDC）的電化學傳感器。利用電化學交流阻抗（EIS）技術對該傳感器進行表征，采用循環伏安法（CV）研究NHDC在ZIF-8/Nafion電極表面的電化學行為，并優化實驗條件。NHDC在ZIF-8/Nafion膜上有靈敏的響應。采用差分脈沖伏安法（DPV）建立了定量檢測NHDC的方法，方法線性范圍為0.16~160 μmol/L，檢出限為56 nmol/L。該方法檢測飲料中NHDC的加標回收率范圍為99.0%~101.3%。
關鍵詞：ZIF-8；電泳沉積法；新橙皮苷二氫查耳酮（NHDC）；電化學傳感器
中圖分類號：TS207.3；O657.1 文獻標識碼：A 文章編號：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
八面體二氧化鈰負載金納米粒子的電化學傳感器檢測鄰氨基苯酚
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. 廣西民族師范學院化學與生物工程學院，光電化學傳感與區域環境分析實驗室，崇左 532200；2. 中國-泰國崇左產業園管理委員會，崇左 532200）
摘要：采用原位生長法制備了八面體二氧化鈰（CeO2）負載金納米粒子（Au NPs）復合材料Au NPs@ CeO2，用掃描電鏡及能量色散X射線光譜儀對復合材料進行形貌表征與元素分析。利用此復合材料修飾玻碳電極，構筑了一種鄰氨基苯酚電化學傳感器。CeO2性質穩定，其八面體結構提供了較大的比表面積，Au NPs具備極佳的導電性，二者復合協同發揮良好的電催化能力。研究發現，Au NPs@CeO2復合材料修飾電極對鄰氨基苯酚表現出較高的檢測靈敏度，在優化實驗條件下，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濃度范圍內呈現2段較好的線性關系，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。該電化學傳感器用于實際樣品中鄰氨基苯酚的測定，回收率為98.0%~105.3%，相對標準偏差為0.9%~3.1%。
關鍵詞：二氧化鈰；金納米粒子；電化學傳感器；鄰氨基苯酚
中圖分類號：O657.1 文獻標識碼：A 文章編號：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-高效液相色譜法測定環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，高樹林*，葛丹丹
（昆明學院化學化工學院，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-高效液相色譜聯用檢測柯衣定、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）和量子化學計算研究DESs的形成機理。對DESs組成、萃取溶劑體積、萃取時間、溶液pH和鹽濃度等實驗條件進行了優化。在最優化條件下，柯衣定、金胺O和羅丹明B在5~1000 ng/mL范圍內線性關系良好，相關系數均大于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環境水樣和飲料樣品中的金胺O、羅丹明B和柯衣定，加標回收率為85.7%~106.8%，相對標準偏差為0.2%~7.7%。
關鍵詞：疏水性低共熔溶劑；模擬計算；合成色素；分散液-液微萃??；高效液相色譜法
中圖分類號：O661.1 文獻標識碼：A 文章編號：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化平臺
劉晨曦，姚延祿，周新麗*
（上海理工大學健康科學與工程學院，上海 200093）
摘要：基于磁珠法核酸提取原理，設計并制作出旋轉驅動式核酸提取微流控芯片及自動化平臺。微流控芯片包括裂解腔、清洗腔以及洗脫腔等結構，步進電機帶動微流控芯片旋轉，通過電磁鐵吸附微流控芯片內的磁珠，實現磁珠在各腔室轉移，完成核酸提取和純化。對芯片表面疏水性、磁力大小、磁珠分散程度以及核酸洗脫時間進行優化。結果表明，當磁力大小為250 N時，可實現磁珠轉移；磁鐵放置于芯片上方1 mm時，腔室內磁珠分散程度最好。洗脫時間為20 min時，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相結合提取的核酸樣本，可直接應用于后續聚合酶鏈式反應擴增環節，有利于實現核酸自動提取及擴增的一體化。
關鍵詞：微流控技術；核酸提??；磁珠法；自動化提取
中圖分類號：R331 文獻標識碼：A 文章編號：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用
薛俊萍，魏國，柴佩君，吳文璞，張異夢，李桂生*，宋志花*
（新型制劑與生物技術藥物研究山東省高校協同創新中心，分子藥理和藥物評價教育部重點實驗室，煙臺大學藥學院，煙臺 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，應用廣泛，其準確定量具有重要意義。近年來，基于分子印跡技術合成的分子印跡聚合物（MIPs）備受關注。MIPs可模擬酶與底物或抗體與抗原之間的相互作用，對目標物進行高選擇性識別。將MIPs應用于核苷類藥物分離分析過程，可顯著提高選擇性和檢測靈敏度。本文對近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中的應用進行綜述，總結了檢測過程中面臨的挑戰，并對其應用前景進行了展望。
關鍵詞：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：O657.31；X832 文獻標識碼：A 文章編號：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
基于智能手機現場快速檢測技術研究進展
唐博1，陳佳敏1，韓永輝*1，2，崔建升*1，劉大喜1
（1. 河北科技大學環境科學與工程學院，石家莊 050018；2. 河北省固體廢棄物資源化技術創新中心，石家莊 050018）
摘要：作為一種便攜式的功能性移動電子設備，智能手機的廣泛應用為便攜式檢測提供了發展平臺，并在臨床診斷、食品安全分析和環境監測等領域表現出巨大的應用潛力。本文綜述了2018~2022年，基于智能手機與比色法、熒光法、化學發光法、電化學分析、免疫分析及微流控分析等技術聯用的即時檢測應用研究進展，并對其發展趨勢和應用前景進行了展望。
關鍵詞：智能手機；即時檢測；綜述
中圖分類號：O657 文獻標識碼：A 文章編號：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研究進展
謝以清1，2，符鴿3，閏凌君1，閆萌萌1，2，雷海民2，馬強*1
（1. 中國檢驗檢疫科學研究院，北京 100176；2. 北京中醫藥大學中藥學院，北京102488；3. 中國消費品質量安全促進會，北京 100125）
摘要：藥食同源中藥材具有營養和藥用的雙重價值，因此被廣泛應用于食品、醫藥等領域。藥食同源中藥材鑒定是藥食同源中藥材應用的基礎。近年來，隨著各學科內容和方法的豐富和創新，藥食同源中藥材鑒定技術也得到了發展，涌現出一些新的技術和方法。同時，多元化的現代鑒定技術和傳統鑒定技術形成了相互補充、相互促進的關系，有利于研究制定規范化的藥食同源中藥材質量標準，并推動中醫藥的現代化、科學化、國際化創新發展。本文介紹了藥食同源中藥材的歷史背景和發展現狀，總結了傳統經驗鑒定、分子生物學鑒定、光譜鑒定、色譜-質譜聯用鑒定等各種鑒定技術的特點和優勢，對國內外新技術、新方法的應用進行了重點闡述，并對藥食同源中藥材鑒定技術的發展趨勢進行了展望，以期為相關領域技術人員提供參考。
關鍵詞：藥食同源中藥材；鑒定技術；研究進展
中圖分類號：R282.5 文獻標識碼：A 文章編號：1000-0720（2024）01-0139-10
Research progress of identification techniques on medicinal and edible traditional Chinese medicine
XIE Yiqing1，2，FU 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
