CuNCs荧光探针检测环境水样中的孔雀石绿

刘梅¹，林洪¹，吴云英¹，胡栋宝¹，伍贤学¹，余琴¹，陈文静^*1，谢建新^*2

（1. 玉溪师范学院化学生物与环境学院，玉溪 653100；2. 黔南民族师范学院化学化工学院，都匀 55800）

摘要：以Cu（NO₃）₂为原料，D-青霉胺（DPA）为还原剂和稳定剂，采用一锅法在室温下制备出高量子产率的红色荧光铜纳米簇（CuNCs），构建了一种可简单快速检测孔雀石绿（MG）的荧光探针。优化了CuNCs的合成条件，采用透射电子显微镜（TEM）、X射线光电子能谱（XPS）、傅里叶变换红外光谱（FT-IR）对CuNCs的形貌及组成进行了表征。MG对CuNCs具有选择性猝灭效应，在1~75 μmol/L浓度范围内，MG的浓度与CuNCs的荧光强度（F₀/F）呈良好的线性关系，检出限为0.75 μmol/L。该荧光探针成功用于湖水中MG的灵敏检测，加标回收率为99.1%~109.9%。该方法可用于环境水样中MG的高灵敏检测。

关键词：铜纳米簇；孔雀石绿；荧光猝灭

中图分类号：O657.3    文献标识码：A    文章编号：1000-0720（2023）10-1279-06

CuNCs fluorescent probe for the detection of malachite green in environmental water samples

LIU Mei¹，LIN Hong¹，WU Yunying¹，HU Dongbao¹，WU Xianxue¹，YU Qin¹，CHEN Wenjing^*1，XIE Jianxin^*2

1. School of Chemistry，Biology and Environment，Yuxi Normal University，Yuxi 653100，China；2. School of Chemistry and Chemical Engineering，Qiannan Normal University for Nationalites，Duyun 55800，China）

Abstract：Using copper nitrate as raw material and D-penicillamine （DPA） as reducing and stabilizing agent，red fluorescent copper nanoclusters （CuNCs） with high quantum yield were prepared by one-pot method at room temperature，and then a fluorescent probe for simple and rapid detection of malachite green （MG） was established. The synthesis conditions were optimized，and the morphology and composition of CuNCs were characterized by transmission electron microscope （TEM），X-ray photoelectron spectroscopy （XPS） and Fourier transform infrared spectrometer （FT-IR）. The fluorescence of CuNCs could be selectively quenched by MG. The fluorescence intensity of CuNCs （F₀/F） had a good linear relationship with the concentration of MG in the range of 1-75 μmol/L，and the detection limit was as low as 0.75 μmol/L. The fluorescence probe was successfully used for the sensitive detection of MG in lake water，and the recoveries were 99.1%-109.9%. The proposed method could be applied for highly sensitive detection of MG in environmental water samples.

Keywords：copper nanoclusters （CuNCs）；malachite green （MG）；fluorescence quenching 

微型近红外光谱法快速检测赛买提杏糖度

彭娟¹，邵学广^*2，楚刚辉^*1

（1. 新疆特色药食用植物资源化学实验室，喀什大学化学与环境科学学院，喀什 844000；2. 南开大学化学学院分析科学研究中心，天津 300071）

摘要：为实现赛买提杏糖度（SSC）的快速检测，并建立一个稳健的预测模型，本文使用微型近红外光谱仪采集光谱，数显糖度计测定SSC，对比了连续小波变换（CWT）、卷积平滑（SG）、多元散射校正（MSC）、标准正态变换（SNV）、一阶导（1^st），二阶导（2^nd）及其两两组合的光谱预处理方法建模结果，结果显示，CWT，CWT+MSC和CWT+SNV 3种方法结果较好。以这3种预处理方法为基础，对比了竞争自适应加权抽样（CARS）、随机化试验（RT）、蒙特卡罗-无信息变量消除法（MC-UVE）和C值法4种变量选择方法，分别得出与杏糖度相关的光谱变量，建立了赛买提杏糖度偏最小二乘（PLS）预测模型，经CWT+MSC光谱预处理加C值法变量选择建立的PLS模型最佳，其预测相关系数（R_p）从0.844优化到0.960，预测均方根误差（RMSEP）从1.273降低到0.699，相对分析偏差（RPD）从1.853上升到3.430。结果表明，适当光谱预处理和变量选择能有效提高赛买提杏糖度快速无损检测的效率和准确性。

关键词：赛买提杏；变量选择；近红外光谱；糖度

中图分类号：O657.3    文献标识码：A    文章编号：1000-0720（2023）10-1285-07

Rapid detection of Cymaiti apricot soluble 

solids content by miniature near infrared spectroscopy

PENG Juan¹，SHAO Xueguang^*2，CHU Ganghui^*1

1. Chemistry Laboratory of Xinjiang Special Medicinal Edible Plant Resources，College of Chemistry and Environmental Science，Kashi University，Kashi 844000，China；2. Analytical Science Research Center，School of Chemistry，Nankai University，Tianjin 300071，China）

Abstract：To realize the rapid detection of Cymaiti apricot soluble solids content （SSC） and establish a steady prediction model of SSC，a miniature near-infrared spectrometer was used to collect the spectra，and a digital display sugar meter was used to determine the SSC.Then the modeling results including continuous wavelet transform（CWT），Savitzky-Golay（SG smoothing），multiplicative scatter correction（MSC），standard normal variate（SNV），firstderivative（1^st），second derivative（2^nd） and the spectral pretreatment method of two combinations were compared，and the models of CWT，CWT+MSC and CWT+SNV showed good results. Based on above three pretreatment methods，four variable selection methods including competitive adaptive reweighted sampling （CARS），randomization test （RT），informative variables elimination （MC-UVE） and C value were compared by obtaining the spectral variables related to SSC of apricot. And the partial least squares （PLS） prediction model of apricot SSC was established. The best model was established by CWT+MSC peretreatment combined with C value variable selection method. The correlation coefficient （R_p） of prediction set increased from 0.844 to 0.960，the root mean square error of prediction （RMSEP） set decreased from 1.273 to 0.699，and the relative percent deviation （RPD） increased from 1.853 to 3.430.The results showed that spectral pretreatement and variable selection properly could effectively improve the efficiency and accuracy of the portable and rapid nondestructive testing of apricot SSC.

Keywords：Cymaiti apricot；variable selection；near infrared spectroscopy；soluble solids content （SSC）

破乳诱导萃取食用植物油中营养元素的原子发射光谱分析

李爱阳¹，陈宇¹，殷子懿¹，黄建华^*2

（1. 湖南工学院化学与环境工程学院，衡阳 421002；2. 湖南省中医药研究院中药研究所，长沙 410013）

摘要：基于破乳诱导萃取，提出利用微波等离子体原子发射光谱（MP-AES）测定食用植物油中多种营养元素的新策略。采用5%（w/V）的Triton X‐114为乳化剂，50%（V/V）的HCl为萃取剂，对食用植物油样品于90 ℃下超声水浴40 min，将分析元素从有机基质转移至酸性水相，采用MP-AES测定其中的8种营养元素（K，Na，Ca，Mg，Fe，Mn，Cu，Zn）。8种元素在各自质量浓度范围内呈良好的线性关系，线性相关系数（R）≥0.9998，检出限（LOD）在0.16~1.95 μg/L之间，样品的加标回收率在94.0%~105.0%之间，相对标准偏差（RSD）≤4.0%。本方法测定结果与国标法基本一致。应用所建立的方法对市场上不同产地的花生油、玉米油、油菜籽油、山茶油、葵花籽油和橄榄油进行检测，6种食用植物油中富含8种营养元素。本方法已用于食用植物油中营养元素的质量评价。

关键词：破乳诱导萃取；食用植物油；微波等离子体原子发射光谱；营养元素

中图分类号：O657.31    文献标识码：A    文章编号：1000-0720（2023）10-1292-07

Determination of nutrient elements in edible vegetable oil 

by atomic emission spectroscopy based on extraction induced by emulsion breaking

LI Aiyang¹，CHEN Yu¹，YIN Ziyi¹，HUANG Jianhua^*2

1. Department of Chemical and Environmental Engineering，Hunan Institute of Technology，Hengyang 421002，China；2. Institute of Chinese Materia，Hunan Academy of Traditional Chinese Medicine，Changsha 410013，China）

Abstract：A new strategy for the determination of multiple nutrient elements in edible vegetable oil using microwave plasma atomic emission spectroscopy （MP-AES） was proposed based on the extraction induced by emulsion breaking. Using 5% （w/V） Triton X-114 as emulsifier and 50% （V/V） hydrochloric acid as extractant，the edible vegetable oil samples were subjected to ultrasonic water bath at 90 ℃ for 40 min，leading to the analytes transferred from organic matrix to acidic aqueous phase. The eight kinds of nutrient elements （K，Na，Ca，Mg，Fe，Mn，Cu and Zn） were determined by MP-AES. The linear correlation coefficients of the analytes in their respective mass concentration ranges were no less than 0.9998，showing good linear relationships. The limits of detection （LODs） were 0.16-1.95 μg/L，and the spiked recoveries were 94.0%-105.0%，with the relative standard deviations （RSDs） no higher than 4.0%. The results of this method were basically consistent with that of the standard method. The developed method was used to detect nutrient elements in peanut oil，corn oil，rapeseed oil，camellia oil，sunflower oil and olive oil from different origins in the domestic market. The results showed 6 kinds of edible vegetable oils were rich in 8 kinds of nutrient elements. The method has been used for the quality evaluation of nutrient elements in edible vegetable oil.

Keywords：extraction induced by emulsion breaking；edible vegetable oil；microwave plasma atomic emission spectroscopy；nutrient elements

复合纳米酶传感器可视化检测水中汞离子

赵凤霞^1，2，李丹靓^1，2，陈果¹，邵飞¹，刘思汝¹，严杭丽^1，2，郑毅^1，2，杨胜园^*1，2，梁好^*1，2

（1. 南华大学衡阳医学院，衡阳 421001；2. 衡阳市健康危害因子检验检疫新技术研究重点实验室，衡阳 421001）

摘要：基于贵金属银修饰的单壁碳纳米管（Ag-SWNTs）复合纳米酶的催化作用及L-半胱氨酸（L-Cys）和汞离子（Hg²⁺）的特异性结合作用，建立了一种快速检测Hg²⁺的可视化比色方法。在适宜的pH条件下，当Hg²⁺不存在时，L-Cys可抑制Ag-SWNTs酶活性，使得3，3’，5，5’-四甲基联苯胺（TMB）无法被催化氧化显色；而当Hg²⁺存在时，Hg²⁺可特异性结合L-Cys，Ag-SWNTs的酶活性不被抑制，TMB被催化氧化为oxTMB，溶液颜色发生由无色至蓝色的变化。在最佳实验条件下，该检测体系在最大吸收波长653 nm处的吸光度值与1.35~90.91 μg/mL范围内的Hg²⁺浓度呈良好的线性关系，回归方程为ΔA=0.0076c-0.085，相关系数是0.9930，检出限为0.44 μg/mL。该方法应用于环境水中Hg²⁺的测定，加标回收率为92.4%~99.9%。

关键词：单壁碳纳米管；L-半胱氨酸；汞离子检测；纳米酶；催化作用

中图分类号：R115    文献标识码：A    文章编号：1000-0720（2023）10-1299-05

Visual detection of mercury ions based on composite nano-enzyme sensor

ZHAO Fengxia^1，2，LI Danliang^1，2，CHEN Guo¹，SHAO Fei¹，LIU Siru¹，YAN Hangli^1，2，ZHENG Yi^1，2，YANG Shengyuan^*1，2，LIANG Hao^*1，2

1. Hengyang Medical School，University of South China，Hengyang 421001，China；2. Key Laboratory of Hengyang for Health Hazard Factors Inspection and Quarantine，Hengyang 421001，China）

Abstract：A new colorimetric method was established for the rapid visual detection of Hg²⁺ based on the catalysis of silver modified single wall carbon nanotubes （Ag-SWNTs） and the specific binding of L-Cys and mercury ions （Hg²⁺）. In the absence of Hg²⁺ at appropriate pH，L-gystein （L-Cys） can inhibit the enzymatic activity of Ag-SWNTs to catalyze the chromogenic reaction of 3，3'，5，5'-tetramethylbenzidine （TMB）. while in the presence of Hg²⁺，Hg²⁺ can specifically bind to L-Cys to keep the enzymatic activity of Ag-SWNTs，TMB was catalyzed and oxidized to oxTMB，and the color of the solution changed from colorless to blue. Under the optimal experimental conditions，the absorbance value of the detection system at the maximum absorption wavelength of 653 nm had a good linear relationship with the concentration of Hg²⁺ in the range of 1.35-90.91 μg/mL，and the linear regression equation was ΔA=0.0076c-0.085，with the relative correlation coefficient （r） of 0.9930. The limit of detection （LOD） for Hg²⁺ was 0.44 μg/mL. This method can be applied to determine Hg²⁺ in environmental water，and the recoveries for spiking experiments were 92.4%-99.9%.

Keywords：single-walled carbon nanotube；L-cysteine；the detection of mercury ions；nano-enzyme；catalytic action

超声法制备环糊精-铂纳米酶并用于检测葡萄糖

姜翠凤^*1，2，王金山¹，阮志凡¹，熊芳芳¹，刘星宇¹，刘艺媛¹，郭伟¹

（1. 盐城工学院材料科学与工程学院，盐城 224051；2. 盐城工学院江苏省生态环境材料重点实验室，盐城 224051）

摘要：通过超声辅助法制备了具有类过氧化物酶、类氧化物酶和类过氧化氢酶活性的β-环糊精-铂纳米粒子（CD-PtNPs），该纳米材料在同一酸度条件下同时具有3种类酶活性。对影响其类过氧化物酶活性的因素进行了优化，最佳条件为：温度20 ℃，pH 3.6，3，3’，5，5’-四甲基联苯胺（TMB）浓度2 mmol/L，H₂O₂ 浓度78 μmol/L，CD-PtNPs用量0.648 μg。基于其类过氧化物酶活性，构建了可通过比色和紫外可见吸收光谱检测葡萄糖的传感平台。该传感平台在缓冲溶液中对葡萄糖的检出限为80 μmol/L，在30%（V/V）血清中检出限为0.18 mmol/L。CD-PtNPs制备方法简便、快速且可避免聚集，有望在生物分析领域得到广泛应用。

关键词：超声辅助合成；纳米酶；铂纳米材料；葡萄糖；传感器

中图分类号：O657.31；X832    文献标识码：A    文章编号：1000-0720（2023）10-1304-07

Ultrasound-assisted synthesis of 

β-cyclodextrin-platinum nanozyme and its application for glucose detection

JIANG Cuifeng^*1，2，WANG Jinshan¹，RUAN Zhifan¹，XIONG Fangfang¹，LIU Xingyu¹，LIU Yiyuan¹，GUO Wei¹

1. School of Materials Science and Engineering，Yancheng Institute of Technology，Yancheng 224051，China；2. Key Laboratory for Ecological-Environment Materials of Jiangsu Province，Yancheng Institute of Technology，Yancheng 224051，China）

Abstract：β-cyclodextrin-platinum nanoparticles （CD-PtNPs） with peroxidase-，oxidase- and catalase-like activity were prepared by an ultrasound-assisted reduction method. The optimal conditions for peroxidase-like activity were as follows：20 ℃，pH 3.6，2 mmol/L of TMB，78 μmol/L of H₂O₂ and 0.648 μg of CD-PtNPs. Based on the excellent peroxidase-like activity，the limit of detection （LOD） for glucose was of 80 μmol/L. Furthermore，this method allowed rapid detection of glucose in 30% （V/V） serum with LOD of 0.18 mmol/L. This ultrasound-assisted method could be expanded to prepare other kind of nanozymes，and CD-PtNPs were expected to have wide application in bioanalytical chemistry.

Keywords：ultrasound-assisted synthesis；nanozyme；Pt nanoparticles；glucose；sensor

一种基于香豆素的荧光探针的合成及其对铝离子和锌离子的识别

李娜，李政^*，王树军，陈钰，肖立伟

（廊坊师范学院化学与材料科学学院，廊坊 065000）

摘要：设计合成了以4-甲基-7-羟基-8-醛基香豆素为荧光团，4-氨基安替比林为识别位点的探针ACAP，通过红外光谱、核磁共振氢谱及碳谱对探针的结构进行了表征。利用荧光光谱研究了探针对不同金属离子的识别性能。结果显示，在CH₃OH/Tris-HCl（9∶1，V∶V）缓冲溶液中，探针ACAP对Al³⁺和Zn²⁺具有选择性识别及良好的识别灵敏性。离子竞争实验显示，其它共存离子对探针识别Al³⁺/Zn²⁺几乎没有影响，表明探针具有良好的抗干扰性。结合比测试显示，探针ACAP与Al³⁺和Zn²⁺均以1∶1结合。探针ACAP对Al³⁺和Zn²⁺的检出限分别为1.78 μmol/L和0.194 μmol/L，均低于世卫组织（WHO）对饮用水中Al³⁺和Zn²⁺所允许的最高浓度。

关键词：香豆素；铝离子；锌离子；荧光探针；性能

中图分类号：O657.31；X832    文献标识码：A    文章编号：1000-0720（2023）10-1311-06

Synthesis and properties of a coumarin-based

 fluorescent probe for the detection of Al³⁺ and Zn²⁺

LI Na，LI Zheng^*，WANG Shujun，CHEN Yu，XIAO Liwei

College of Chemistry and Materials Science，Langfang Normal University，Langfang 065000，China）

Abstract：A probe ACAP was designed and synthesized using 4-methyl-7-hydroxy-8-uronic coumarin as fluorophore and 4-amino-antipyrine as recognition site. The structure of the probe was characterized by infrared spectrum，¹H-NMR and ¹³C-NMR spectra. The recognition performance of the probe for different metal ions was investigated by fluorescence spectroscopy. The results showed that the probe ACAP had a selective recognition and a good sensitivity to Al³⁺ and Zn²⁺ in CH₃OH/Tris-HCl （9∶1，V∶V） buffer solution. Ion competition experiments revealed that other co-existing ions had little effects on Al³⁺/Zn²⁺ recognition，indicating that the probe possessed a good anti-interference. Binding ratio test manifested that the probe ACAP bond with Al³⁺/Zn²⁺ in a 1∶1 manner. The detection limits for Al³⁺ and Zn²⁺ were estimated to be 1.78 μmol/L and 0.194 μmol/L，respectively，which were lower than the permissible concentrations of Al³⁺ and Zn²⁺ described by World Health Organization （WHO） in drinking water.

Keywords：coumarin；Al³⁺；Zn²⁺；fluorescence probe；properties

基于三螺旋适体探针的双向开关传感同时灵敏测定四环素和氯霉素

王子棋，高亚芳，谭心韵，李安祺，鲁理平^*

（北京工业大学环境科学系，区域大气复合污染防治北京市重点实验室，北京100124）

摘要：设计了基于发卡状三螺旋结构的DNA分子开关荧光传感器，利用适配体特异性识别，实现了对2种目标抗生素的同时灵敏测定。其分子开关结构由一个特异性适配体识别序列和一个双标记的信号探针序（STP）列组成发卡状三螺旋结构。识别四环素的STP两端用芘分子修饰，识别氯霉素的信号探针两端分别用硫化镉量子点（CdS QDs）和金纳米粒子（AuNPs）修饰，适配体序列插入环状（Loop）区域形成三链结构。目标抗生素存在时，识别探针与之结合，释放出信号探针，致使两端发光物质靠近，荧光信号发生显著变化。传感器的荧光发光强度与四环素和氯霉素浓度呈良好的线性关系，线性范围为1×10^-3~10 μmol/L，检出限为0.3 nmol/L。该方法用于测定鸡蛋中的四环素和氯霉素，结果满意。

关键词：四环素；氯霉素；三螺旋DNA；分子开关；荧光传感器

中图分类号：O657.3    文献标识码：A    文章编号：1000-0720（2023）10-1317-07

Simultaneous and sensitive determination of tetracycline 

and chloramphenicol by two-way switch sensing based on triple helix aptamer probe

WANG Ziqi，GAO Yafang，TAN Xinyun，LI Anqi，LU Liping^*

Key Laboratory of Beijing on Regional Air Pollution Control，Faculty of Environment Science，Beijing University of Technology，Beijing 100124，China）

Abstract：A DNA molecular switch fluorescence sensor based on hairpin triple helix structure was designed to achieve simultaneous sensitive determination of two target antibiotics by aptamer specific recognition. The molecular switching structure consists of a specific aptamer recognition sequence and a double-labeled signal probe sequence. The two ends of the signal probe for tetracycline recognition were modified with pyrene molecules，and the two ends of the signal probe for chloramphenicol recognition were modified with cadmium sulfide quantum dots （CdS QDs） and gold nanoparticles，respectively. The aptamer sequence was inserted into the loop region to form a three-chain structure. When the target antibiotic was present，the recognition probe bound to it and released a signal probe，bringing the luminescent substance at both ends closer together，and the fluorescence signal changed significantly （enhanced or reduced）. The fluorescence intensity of the sensor showed a good linear relationship with the concentrations of tetracycline and chloramphenicol，the linear range was 1×10^-3-10 μmol/L，and the detection limit was 0.3 nmol/L. The method was used to determine tetracycline and chloramphenicol in eggs with satisfactory results.

Keywords：tetracycline；chloromycetin；triple-helix DNA；molecular switch；fluorescence sensor

毛细管内标定量核磁共振波谱法测定滴眼液中氧氟沙星含量

曾贝怡¹，史丹阳¹，刘兆鑫¹，郭强胜¹，李静²，许旭^*1

（1. 上海应用技术大学化学与环境工程学院，上海 201418；2. 上海通微分析技术有限公司，上海 201203）

摘要：建立了一种毛细管内标封管的定量核磁共振波谱（qNMR）法测定滴眼液中氧氟沙星的含量。将内标物邻苯二甲酸氢钾溶于氘代试剂重水并预先封入毛细管中，分别用已知含量的3种纯品测定其校正因子（k）为0.03125±0.00033，该值稳定且与样品无关，可直接用于测定其他成分。将其用于测定滴眼液样品中氧氟沙星的含量，以δ 1.53 ppm （H-14，d，J=6.5 Hz，3H）为定量峰。实验结果表明，氧氟沙星浓度和氧氟沙星与内标定量峰面积比值呈线性关系，线性相关系数为0.9999，检出限为0.03 mg/mL。方法日内相对标准偏差（RSD）为0.5%，加标回收率为98.8%~103.9%。本方法操作简便、结果准确，减少了内标与氘代试剂的用量。

关键词：定量核磁共振波谱法；毛细管内标；氧氟沙星；滴眼液

中图分类号：O657.2    文献标识码：A    文章编号：1000-0720（2023）10-1324-08

Determination of ofloxacin in eye drops by quantitative 

nuclear magnetic resonance spectroscopy using capillary internal standard

ZENG Beiyi¹，SHI Danyang¹，LIU Zhaoxin¹，GUO Qiangsheng¹，LI Jing²，XU Xu^*1

1. School of Chemical and Environmental Engineering，Shanghai Institute of Technology，Shanghai 201418，China；2. Unimicro （Shanghai） Technologies Co.，Ltd.，Shanghai 201203，China）

Abstract：A quantitative nuclear magnetic resonance spectroscopy （qNMR） method using capillary internal standard was presented and applied for the determination of ofloxacin in eye drops. The internal standard of potassium hydrogen phthalate was dissolved in deuterium reagent and pre-sealed into a capillary. The internal standard capillary was placed into a nuclear magnetic tube containing the sample and used for qNMR determination. The correction factor （k） of an internal standard capillary was detected as 0.03125±0.00033 using 3 kinds of pure compounds with known contents. The k value was stable and independent of the sample，and could be applied for the direct determination of other components. For the qNMR determination of ofloxacin content in eye drops，the peak at δ 1.53 ppm （H-14，d，J=6.5 Hz，3H） was selected as the quantitative peak. The results showed that the correlation coefficient was 0.9999 for the linear curve between ofloxacin concentration and the peak area ratio of ofloxacin to internal standard，and the limit of detection （LOD） was 0.03 mg/mL. The relative standard deviation （RSD） of the method was 0.5%，and the recoveries were 98.8%-103.9%. The qNMR method using internal standard sealed capillary tube was simple and accurate，and decreased the consumption of internal standard and deuterium reagents.

Keywords：quantitative nuclear magnetic resonance spectroscopy；capillary internal standard；ofloxacin；eye drops

两阶段相关系数波长选择方法

万岩¹，陈争光^*1，焦峰²

（1. 黑龙江八一农垦大学信息与电气工程学院，大庆 163319；2. 黑龙江八一农垦大学农学院，大庆 163319）

摘要：为降低建立模型的复杂度，提高近红外光谱模型的预测精度，提出一种两阶段相关系数（TSCC）波长选择方法。先计算各波长点向量和浓度向量之间的相关系数，选择相关系数较大的波长点作为第一阶段波长。在此基础上计算各个波长点之间的相关系数，选择与其他波长点之间相关系数较小的波长作为建模波长。采用2组公开数据集对算法进行验证，在第一阶段波长选择结果和两阶段波长选择结果上分别建立偏最小二乘回归（PLSR）模型和多元线性回归（MLR）模型。结果表明，基于TSCC波长选择算法建立的MLR模型（TSCC-MLR），性能优于基于全谱的PLSR模型（Full-PLSR）、优于基于第一阶段波长选择结果建立的PLSR模型（CC-PLSR）和基于连续投影算法（SPA）选择的数据建立的MLR模型（SPA-MLR）。玉米数据SPA-MLR模型决定系数R²为0.8353，CC-PLSR模型R²为0.8652，TSCC-MLR模型R²为0.8951。土壤样本的近红外光谱数据集，基于TSCC算法提取变量后，得到18个特征波长并建立MLR模型，R²达到0.9688，相较于CC-PLSR和SPA-MLR模型，模型预测性能有所提升。通过2个数据集得到的结果，证明了本文所提出的TSCC波长选择方法是一种有效的变量选择方法。

关键词：近红外光谱；特征波长选择；相关系数；多元线性回归

中图分类号：O657.33；S132    文献标识码：A    文章编号：1000-0720（2023）10-1332-09

A wavelength selection method based on two-stage correlation coefficient

WAN Yan¹，CHEN Zhengguang^*1，JIAO Feng²

1. College of Electrical and Information，Heilongjiang Bayi Agricultural University，Daqing 163319，China；2. Agriculture College，Heilongjiang Bayi Agricultural University，Daqing 163319，China）

Abstract：To simplify model construction and increase the precision of near-infrared spectrum （NIRS） prediction models，a two-stage correlation coefficient （TSCC） wavelength selection method was proposed. The correlation coefficient between each wavelength vector and the concentration vector was first calculated，and the wavelength with the larger correlation coefficient was chosen as the result of the first stage wavelength selection. Based on this，the correlation coefficient between each wavelength was calculated，and the modeling wavelength was chosen based on the wavelength with the lowest correlation coefficient to the other wavelengths. The algorithm was validated using two publicly accessible datasets，and models for partial least squares regression （PLSR） and multiple linear regression （MLR） were created on the outcomes of the first stage wavelength selection and the second stage wavelength selection，respectively. According to the findings，the PLSR model based on the outcomes of the first stage wavelength selection （CC-PLSR），the PLSR model based on full spectra （Full-PLSR），and the MLR model based on data selected by the successive projections algorithm （SPA） （SPA-MLR） were all underperformed by the TSCC-MLR，which was the MLR model based on the wavelength selected by TSCC. Based on the corn dataset，the coefficient of determination （R²） of SPA-MLR，CC-PLSR and TSCC-MLR model were 0.8353，0.8652 and 0.8951，respectively. The NIR spectra of soil samples were extracted by TSCC technology to acquire 18 distinctive wavelengths. The MLR model was developed based on these wavelengths，R_p² of 0.9688. Compared with the CC-PLSR model and SPA-MLR model，the prediction performance of MLR model was enhanced. The results of two datasets showed that the two-stage correlation coefficient wavelength selection method proposed in this paper was an effective variable selection method.

Keywords：near infrared spectroscopy；characteristic wavelength selection；correlation coefficient；multiple linear regression

高效液相色谱法测定化妆品中禁用芳香胺1-萘胺和2-萘胺及其盐类

孟宪双¹，牛增元²，罗忻²，刘艺静^1，3，白桦¹，马强^*1

（1. 中国检验检疫科学研究院，北京 100176；2. 青岛海关技术中心，青岛 266109；3. 北京中医药大学中药学院，北京 102488）

摘要：建立了化妆品中禁用芳香胺1-萘胺和2-萘胺同分异构体及其盐类的高效液相色谱分析方法。膏霜和乳液类试样依次经氯化钠破乳、溶剂萃取；水剂类试样直接经超声辅助溶剂萃取。萃取液经Waters Sep-Pak C₁₈固相萃取柱净化后由XBridge BEH Phenyl色谱柱分离，以0.02 mol/L磷酸二氢钠溶液和甲醇为流动相梯度洗脱，二极管阵列检测器测定，检测波长240 nm，外标法定量。在优化的样品前处理和色谱条件下，1-萘胺和2-萘胺实现基线分离，检出限和定量限分别为0.5 μg/kg和1.0 μg/kg，平均回收率为88.7%~107.3%，相对标准偏差为2.3%~6.8%。该方法解决了法规明确而技术空白的问题，适用于化妆品的日常检验及质量控制。

关键词：固相萃取；高效液相色谱法；禁用芳香胺；同分异构体；化妆品

中图分类号：O657.7    文献标识码：A    文章编号：1000-0720（2023）10-1341-06

Determination of prohibited aromatic amines of 1-naphthylamine

 and 2-naphthylamine and their salts in cosmetics by high-performance liquid chromatography

MENG Xianshuang¹，NIU Zengyuan²，LUO Xin²，LIU Yijing^1，3，BAI Hua¹，MA Qiang^*1

1. Chinese Academy of Inspection and Quarantine，Beijing 100176，China；2.Technology Center of Qingdao Customs，Qingdao 266109，China；3. School of Chinese Materia Medica，Beijing University of Chinese Medicine，Beijing 102488，China）

Abstract：A high-performance liquid chromatography （HPLC） method was established for the analysis of the prohibited aromatic amines of 1-naphthylamine and 2-naphthylamine isomers and their salts in cosmetics. The cream and emulsion samples were successively demulsified by sodium chloride and extracted by solvent，while the lotion samples were directly subjected to ultrasound-assisted solvent extraction. And the extracts were purified by a Waters Sep-Pak C₁₈ solid-phase extraction column and separated by an XBridge BEH Phenyl chromatographic column，along with gradient elution using 0.02 mol/L sodium dihydrogen phosphate solution and methanol as mobile phase at detection wavelength of 240 nm with diode array detector，and quantified by external standard method. Under the optimized pretreatment and chromatographic conditions，1-naphthylamine and 2-naphthylamine were baseline separated. The limits of detection and limits of quantitation were 0.5 and 1.0 μg/kg，respectively. The average recoveries were 88.7%-107.3%，and the relative standard deviations were 2.3%-6.8%. The method could solve the problem of clear regulations but technical blank，and is suitable for daily inspection and quality control of cosmetics.

Keywords：solid-phase extraction；high-performance liquid chromatography；prohibited aromatic amines；isomers；cosmetics

天冬氨酸修饰纳米金-纸芯片体系对高半胱氨酸的选择性检测

张剑^1，2，郑志鸿¹，张丹¹，张博^1，2，李文静^1，2，李一冰¹，夏敏珠¹，刘春叶^*1，2

（1. 西安医学院药学院，西安 710021；2. 西安医学院药物研究所，西安 710021）

摘要：建立了以纸芯片为分析平台的高半胱氨酸（Hcy）快速检测新方法。Hcy使天冬氨酸（Asp）修饰的纳米金（Asp-AuNPs）体系发生团聚，溶液由红色逐渐变为蓝色。使用手机拍照记录结果，Photoshop软件分析显色强度。红/蓝通道颜色比值（ΔRed/Blue）与Hcy浓度在0.74~74 μmol/L范围内呈良好线性关系，回归方程为y=0.0704x+0.5445，相关系数（R）为0.9995，检出限为0.37 μmol/L，加标回收率为98.7%~100.3%。共存还原性物质干扰误差在±2%以内。该方法测得人血浆中Hcy含量为（5.52±0.39） μmol/L，符合人体血浆中Hcy浓度参考范围。

关键词：纳米金；微流控纸基分析平台；高半胱氨酸；比色法

中图分类号：O652    文献标识码：A    文章编号：1000-0720（2023）10-1347-04

Selective determination of homocysteine by a paper-based 

assay system using aspartic acid modified gold nanoparticles

ZHANG Jian^1，2，ZHENG Zhihong¹，ZHANG Dan¹，ZHANG Bo^1，2，LI Wenjing^1，2，LI Yibing¹，XIA Minzhu¹，LIU Chunye^*1，2

1. School of Pharmacy，Xi'an Medical University，Xi'an 710021，China；2. Institute of Medicine，Xi'an Medical University，Xi'an 710021，China）

Abstract：A novel method for homocysteine （Hcy） determination on paper-based analytical devices using aspartic acid （Asp） modified gold nanoparticles （Asp-AuNPs） was proposed. Hcy interacts with Asp-AuNPs selectively and leads to the aggregation of Asp-AuNPs after its addition. A color change from red to blue can be observed on the paper-based analytical devices. The results were recorded using a common cell phone and subsequently analyzed by Photoshop software. The ratio of color intensity at red and blue channel （ΔRed/Blue） increased linearly in the Hcy concentration range of 0.74-74 μmol/L，with the relative coefficient （R） of 0.9995. The regression equation was y=0.0704x+0.5445，the limit of detection was 0.37 μmol/L，and the recoveries of this method were 98.7%-100.3%. The interference deviations of coexisting reductive substances to Hcy were in the range of -2% to 2%. The Hcy concentration in human plasma was determined as （5.52±0.39） μmol/L by this method，which was consistent with the reference range of Hcy.

Keywords：gold nanoparticles；micro?uidic paper-based analytical devices；homocysteine；colorimetric assay

低共熔溶剂液液微萃取-高效液相色谱法测定奶茶中3种甲基黄嘌呤类物质

张悦，杨楠，赵思睿，徐凡，谢哲浩，刘彦^*

（河北医科大学药学院，石家庄 050017）

摘要：建立了基于低共熔溶剂（DES）的液液微萃取-高效液相色谱法（HPLC）测定奶茶中可可碱、咖啡因和茶碱含量的方法。制备了8种不同组成的DES，并选择百里酚-辛酸摩尔比为2∶1的DES为萃取溶剂。在优化的样品前处理及色谱条件下，可可碱、咖啡因和茶碱分别在0.1~50.0 μg/mL浓度范围内线性关系良好，相关系数（r）分别为0.9981，0.9988和0.9975，检出限（LOD）分别为0.06，0.05，0.06 μg/mL，加标回收率为93.8%~102.7%，相对标准偏差（RSD）≤3.9%。该方法适用于测定奶茶中可可碱、咖啡因和茶碱的含量。

关键词：低共熔溶剂；甲基黄嘌呤类；奶茶；液液微萃取；样品前处理

中图分类号：X132    文献标识码：A    文章编号：1000-0720（2023）10-1351-06

Deep eutectic solvent based liquid liquid microextraction-high performance 

liquid chromatography for the determination of three kinds of methylxanthines in milky tea

ZHANG Yue，YANG Nan，ZHAO Sirui，XU Fan，XIE Zhehao，LIU Yan^*

School of Pharmacy，Hebei Medical University，Shijiazhuang 050017，China）

Abstract：A method of liquid-liquid microextraction （LLME） based on deep eutectic solvent （DES） combined with high performance liquid chromatography （HPLC） was established to detect the contents of theophylline，theobromine and caffeine in milky tea. 8 kinds of DESs with different composition were prepared，and DES with the molar ratio of 5-methyl-2-isopropylphenol to octanoic acid of 2∶1 was selected as the extraction solvent. Under the optimized conditions，there were good linear relationships of theophylline，theobromine and caffeine in the range of 0.1-50.0 μg/mL，with the correlation coefficients （r） of 0.9981，0.9988 and 0.9975，respectively. The limits of detection （LODs） of theophylline，theobromine and caffeine were 0.06，0.05 and 0.06 μg/mL，and the average recoveries were 93.8%-102.7%，respectively. With the relative standard deviations （RSDs） less than 3.9%. This method can be applied to detect the contents of three kinds of methylxanthines in milky tea.

Keywords：deep eutectic solvent；methylxanthines；milky tea；liquid-liquid microextraction；sample pretreatment

气相色谱-质谱法测定废液样品中化武相关化合物

吴姬娜，刘石磊，李晓森，闫珑，邢中方，杨旸^*

（国民核生化灾害防护国家重点实验室，北京 102205）

摘要：国际禁化武组织（OPCW）每年定期对各缔约国实验室进行分析能力验证，确保指定实验室能够胜任真实样品分析任务。2021年第50次水平考试由OPCW中心实验室进行配样，共配制6个废液样品。采用气相色谱-质谱法对6个考试废液样品进行分析鉴定，最终检出7个化武相关化合物。通过液液萃取、改变色谱固定相选择性等方法，实现了目标物与背景干扰的有效分离；结合电子轰击电离、化学电离、串联质谱分析等方式，完成了目标化合物结构的准确鉴定，所得结果与考试后OPCW发布的添加化合物清单一致。在鉴定的化合物中有2个为新型化武相关化合物，对其进行了质谱碎裂分析，为相关化学战剂降解、洗消的后续研究提供参考。

关键词：化武相关化合物；能力验证；废液样品；气相色谱-质谱法

中图分类号：O657.63    文献标识码：A    文章编号：1000-0720（2023）10-1357-07

Determination of chemical weapons convention-related compounds 

in waste samples by gas chromatography-mass spectrometry

WU Jina，LIU Shilei，LI Xiaosen，YAN Long，XING Zhongfang，YANG Yang^*

State Key Laboratory of NBC Protection for Civilian，Beijing 102205，China）

Abstract：Organization for the Prohibition of Chemical Weapons （OPCW） conducts the official proficiency tests annually among Member States’ laboratories to ensure that the designated laboratories maintain the technical competence for the analysis of authentic samples. Six waste samples were prepared by the OPCW Laboratory for the 50^th proficiency test in 2021. In this paper，all the six waste samples were analyzed by gas chromatography-mass spectrometry，and seven compounds related to the Chemical Weapons Convention were detected. The target chemicals were effectively separated from the background substances by liquid-liquid extraction or column phase selectivity by different stationary phase selection. The structures of the seven compounds were unambiguously identified by the combination of electron ionization，chemical ionization and tandem mass spectrometry modes，and the results were consistent with the spiking chemical list released by OPCW after the test. Among the identified chemicals，there are two novel Chemical Weapon Convention-related chemicals. The fragmentation pathways were presented in details，which may provide useful reference for the subsequent investigation on degradation and decontamination of the related chemical warfare agents.

Keywords：chemical weapons convention-related compounds；proficiency test；waste sample；gas chromatography-mass spectrometry

哌嗪类新精神活性物质BZP及TFMPP拉曼光谱特性研究

吴国萍^*1，2，胡辰辰^1，2，陆腾³，吴元钊⁴

（1. 江苏警官学院刑事科学技术系，南京 210031；2. 江苏省食品药品与环境犯罪检验技术工程研究中心，南京 210031；3. 中国科学院计算机网络信息中心高性能计算技术与应用发展部，北京100083；4. 浙江警察学院刑事科学技术系，浙江省毒品防控技术研究重点实验室，杭州 310051）

摘要：运用密度泛函理论（DFT）优化哌嗪类新精神活性物质1-苄基哌嗪（BZP）和1-（3-三氟甲基苯基）哌嗪（TFMPP）的几何构型，结合实验测得的拉曼谱图对标准品拉曼谱图的振动模式进行指认和归属，并与低浓度样品的表面增强拉曼（SERS）谱图进行比较；使用自制纳米金、NaCl溶液为助剂，优化BZP和TFMPP的SERS检测条件。在最优条件下，BZP和TFMPP的检出限分别为10 ng/mL和1 μg/mL；重复性实验中2种样品的主要特征峰强度相对标准偏差（RSD）分别4.5%~14%和4.0%~16%。运用基于Matlab自行开发的设计分子光谱数据分析系统的BP神经网络模块，对模拟未知样品进行预测，30份BZP样品和26份TFMPP样品的预测值与真实值比值的平均值（AVG）分别为1.21和0.99，RSD分别为22%和14%。本文可为BZP和TFMPP的拉曼检测提供理论依据和快检方法。

关键词：密度泛函理论；表面增强拉曼光谱；BP神经网络；哌嗪类新精神活性物质

中图分类号：O657.37    文献标识码：A    文章编号：1000-0720（2023）10-1364-09

Study of surface enhanced Raman spectroscopy

 of 1-benzylpiperazine and 1-（3-trifluoromethyl phenyl） piperazine

WU Guoping^*1，2，HU Chenchen^1，2，LU Teng³，WU Yuanzhao⁴

1. Department of Criminal Science and Technology，Jiangsu Police Institute，Nanjing 210031，China；2. Jiangsu Provincial Engineering Research Center for Technical and Criminal Inspection of Food，Drug and Environmental Cases，Nanjing 210031，China；3. Department of High Performance Computing Technology and Application Development，Computer Network Information Center，Chinese Academy of Sciences，Beijing 100083，China；4. Key Laboratory of Drug Prevention and Control Technology of Zhejiang Province，Department of Criminal Science and Technology，Zhejiang Police College，Hangzhou 310051，China）

Abstract：Density functional theory（DFT） was used to optimize and calculate the vibrational wavenumbers of new psychoactive piperazines 1-benzylpiperazine （BZP） and 1-（3-trifluoromethyl phenyl） piperazine （TFMPP），and the samples of BZP and TFMPP were tested by Raman and surface enhanced Raman spectroscopy （SERS）. The Raman spectra of standard samples were compared with the surface enhanced Raman spectra of low concentration. The SERS detection conditions of BZP and TFMPP were optimized by using self-made gold nanoparticles and NaCl solution as additives. Under the optimal detection conditions，the detection limits of BZP and TFMPP were 10 ng/mL and 1 μg/mL，and the relative standard deviations （RSDs） of the main characteristic peak intensities were 4.5%-14% and 4.0%-16%，respectively. BP neural network was used to predict the unknown sample concentration. The average values of the ratio between the predicted value and the true value （AVG） of 30 BZP samples and 26 TFMPP samples were 1.21 and 0.99，with the RSDs of 22% and 14%，respectively. In this paper，the theoretical basis and rapid detection methods for BZP and TFMPP were provided.

Keywords：density functional theory；surface enhanced Raman spectroscopy；BP neural network；new psychoactive piperazines

一测多评法测定化妆品中的21种防晒剂

王继双，李莉^*，王海燕^*

（中国食品药品检定研究院，国家药品监督管理局化妆品研究与评价重点实验室，北京 100050）

摘要：基于一测多评法同时测定化妆品中21种防晒剂含量。采用高效液相色谱法检测，以甲醇、四氢呋喃和高氯酸溶液为流动相，梯度洗脱，在C₁₈色谱柱上分离21种防晒剂。选取二苯酮-3为内部参照物，建立其他20种防晒剂的相对校正因子，计算各组分含量。实验结果表明，21种防晒剂在一定质量浓度范围内线性关系良好，各组分在24 h内稳定。一测多评法和外标法测定结果的相对平均偏差均不大于4.25%，2种方法结果的一致性良好。该方法可用于防晒类化妆品防晒剂的测定和质量控制。

关键词：化妆品；防晒剂；一测多评；高效液相色谱

中图分类号：O657.7    文献标识码：A    文章编号：1000-0720（2023）10-1373-07

Analysis of 21 sunscreen agents in cosmetics

with quantitative analysis of multi-components by single marker

WANG Jishuang，LI Li^*，WANG Haiyan^*

National Institutes for Food and Drug Control，Key Laboratory for Researching and Evaluation of Cosmetics of National Medical Products Administration，Beijing 100050，China）

Abstract：A quantitative analysis of multi-components by single marker （QAMS） method for the determination of 21 kinds of sunscreen agents in cosmetics was established. Using methanol，tetrahydrofuran and perchloric acid as mobile phases，21 kinds of sunscreen agents were separated on a C₁₈ column and detected by high performance liquid chromatography （HPLC） with gradient elution. Diphenylketone-3 was selected as the internal reference substance，and the relative correction factors of the other 20 kinds of sunscreen agents were established to calculate the content of each component. The results showed that the 21 kinds of sunscreen agents had good linear relationships within a certain mass concentration ranges，and each component was stable for 24 h. The results of QAMS were close to that of external standard method （ESM），and the relative error was not higher than 4.25%. This method can be used for the determination and quality control of sunscreen agents in cosmetics.

Keywords：cosmetics；sunscreen；quantitative analysis of multi-components by single marker；high performance liquid chromatography

高效邻苯二甲酸新戊二醇聚酯毛细管柱的制备及应用

石昆，秦金平^*，徐国庆，魏昊东

（南京工业大学化工学院，南京 211816）

摘要：用邻苯二甲酸和新戊二醇合成了邻苯二甲酸新戊二醇聚酯，并对其进行了核磁和红外光谱表征，确定了该物质的微观结构。使用超细SiO₂载体水溶液对毛细管柱内壁进行表面粗糙化处理，以邻苯二甲酸新戊二醇聚酯为固定相，配制5 mg/mL的固定液，用静态法涂渍了毛细管色谱柱，制备了0.25 mm×30 m×0.32 μm邻苯二甲酸新戊二醇聚酯毛细管柱。以甲酚、二甲酚异构体的分离能力评价其分离性能。结果表明，邻苯二甲酸新戊二醇聚酯毛细管柱对甲酚、二甲酚异构体具有良好的分离能力，每米理论塔板数在3000左右，其最高使用温度为250 ℃。建立了用于检测高纯度间甲酚、对甲酚的方法。

关键词：邻苯二甲酸新戊二醇聚酯；毛细管色谱；甲酚异构体；二甲酚异构体

中图分类号：O657.7+1    文献标识码：A    文章编号：1000-0720（2023）10-1380-06

Preparation and application of high efficiency

 neopentyl glycol phthalate polyester capillary column

SHI Kun，QIN Jinping^*，XU Guoqing，WEI Haodong

College of Chemical Engineering，Nanjing Technology University，Nanjing 211816，China）

Abstract：Neopentyl glycol phthalate polyester was synthesized from phthalic acid and neopentyl glycol，and its microstructure was characterized by nuclear magnetic resonance （NMR） and infrared radiation （IR）. The inner wall of capillary column was roughened by using ultrafine SiO₂ carrier aqueous solution. The capillary chromatography column （0.25 mm×30 m×0.32 μm） was successfully prepared by static method，using neopentyl glycol phthalate polyester （5 mg/mL） as stationary phase. The separation performance of cresol and xylenol isomers was evaluated. The results showed that the capillary column of neopentyl phthalate had good separation ability for cresol and xylcresol isomers，the number of theoretical plates per meter was around 3000 and the highest operating temperature was 250 ℃. A method for the analysis of m-cresol and p-cresol with high purity was established.

Keywords：neopentyl glycol phthalate polyester；capillary chromatography；cresol isomer；xylenol isomer

化妆品中大麻二酚的检测方法及溯源研究进展

牛可歆¹，赵霞²，廉洁^*1

（1. 中国人民公安大学侦查学院，北京 100038；2. 国家毒品实验室北京分中心，北京 100164）

摘要：大麻二酚（CBD）是大麻的主要成分，因其具有强大的抗炎抗氧、美白保湿等功效，被越来越多地应用到化妆品中，但受CBD来源和安全性问题的影响，我国对其在化妆品领域的应用进行严格管控。CBD主要通过提取大麻植株中的大麻素获得，其复杂的成分和多样的化妆品品类，使得对化妆品中CBD的前处理和分析检测面临巨大的挑战。近年来，已开发出多种化妆品中大麻素的分析方法，液液萃取是最常用的前处理方法，色谱-质谱联用技术是首选的检测方法，同时便携式仪器设备的多种快检方法也有望应用于化妆品中大麻素的检测。本文综述了化妆品中CBD前处理和检验方法的研究进展，并结合CBD的主要来源，探讨了基于上述检验方法的化妆品原料溯源问题，以期为开展相关科学研究提供参考和借鉴。

关键词：大麻二酚；化妆品；色谱-质谱联用技术；大麻素；溯源

中图分类号：O65    文献标识码：A    文章编号：1000-0720（2023）10-1386-09

Advances of detection methods and traceability study of cannabidiol in cosmetics

NIU Kexin¹，ZHAO Xia²，LIAN Jie^*1

1. School of Investigation，People’s Public Security University of China，Beijing 100038，China；2. Beijing Branch of National Drug Laboratory，Beijing 100164，China）

Abstract：Cannabidiol （CBD） is the main component of cannabis. Because of its powerful anti-inflammatory，antioxidant，whitening and moisturizing effects，it is increasingly used in cosmetics. However，due to the source of CBD and safety issues，China imposes strict controls on its cosmetics sector. CBD in cosmetics mainly comes from extraction of cannabinoids plants. The complexity of its components and the diversity of cosmetic categories make the pretreatment analysis and detection of CBD in cosmetics face huge challenges. In recent years，a variety of analytical methods for detection of cannabinoids in cosmetics have been developed. Liquid-liquid extraction is the most used pretreatment method，and chromatography-mass spectrometry is the preferred laboratory analysis method. With portable instruments and equipment used，a variety of rapid detection methods are also expected to be applied to the detection of cannabinoids in cosmetics. This paper compares the existing detection technologies for detection of cannabinoids in cosmetics，and refers to the idea of chemical typing of cannabis plants，discusses the application of existing detection technologies in the traceability of components，and prospects for the development direction of cannabinoid detection，providing reference for related scientific research.

Keywords：cannabidiol；cosmetics；chromatography-mass spectrometry；cannabinoids；tracing

检测SARS-CoV-2抗体的电化学免疫传感器抗原固定方法研究进展

潘艺文¹，王钰结¹，陈晓雯¹，张晓敏¹，霍朝晖^*1，2

（1. 广东第二师范学院化学与材料科学学院，广州 510303；2. 广东省普通高校先进材料与节能减排工程技术开发中心，广州 510303）

摘要：SARS-CoV-2的免疫球蛋白M和G（IgM和IgG）抗体检测在新型冠状病毒肺炎（COVID-19）的病情分析和诊断监测等方面具有重要意义。电化学免疫传感器作为一种高效的检测工具，可以很好地满足COVID-19抗体诊断的需求，与传统的分子学和血清学抗体检测方法相比，表现出优异的性能，且具有现场快检能力。决定电化学生物传感器检测抗体性能的关键技术是其基底电极的修饰材料和电极表面生物活性分子的固定化技术。本文以电化学生物免疫传感器的设计为基础，综述了基底电极的修饰材料和功能性生物活性分子在电极表面的固定化方式，并对未来SARS-CoV-2抗体检测的电化学免疫传感器的研发进行展望，旨在为增强电化学生物免疫传感器性能和应用价值提供研究思路。

关键词：SARS-CoV-2抗体；电化学；传感器；构建

中图分类号：O657.3；G353.11    文献标识码：A    文章编号：1000-0720（2023）10-1395-11

Research progress of antigen fixation methods

 of electrochemical immunosensor for detecting SARS-CoV-2 antibodies

PAN Yiwen¹，WANG Yujie¹，CHEN Xiaowen¹，ZHANG Xiaomin¹，HUO Zhaohui^*1，2

1. School of Chemistry and Materials Science，Guangdong University of Education，Guangzhou 510303，China；2. Engineering Technology Development Center of Advanced Materials & Energy Saving and Emission Reduction in Guangdong Colleges and Universities，Guangzhou 510303，China）

Abstract：The detection of SARS-CoV-2 Immunoglobulin M（IgM） and Immunoglobulin G（IgG） antibodies is of great significance in disease analysis，diagnosis and surveillance of COVID-19. As an highly effective detection tool，electrochemical immunosensors can well meet the needs of COVID-19 antibodies diagnosis. Compared with traditional molecular and serological antibodies detection methods，it shows excellent performance and has the ability of rapid onsite detection. The performance of electrochemical biosensors depends on the modification material on the electrode substrate and the immobilization technology of bioactive molecules on the electrode surface. Based on the design of the electrochemical bioimmunosensors，the immobilization methods of the modification material on the electrode substrate and the functional bioactive molecules on the electrode surface are reviewed，and the development of electrochemical immunosensors for detecting SARS-CoV-2 antibody in the future is prospected，aiming to provide research ideas for enhancing the performance and application of electrochemical bioimmunosensors.

Keywords：SARS-CoV-2 antibody；electrochemistry；sensor；construction

硫化氢中毒检验技术研究进展

张震¹，张云峰²，吴小军^*1，2，王继芬¹，鲁朋武³

（1. 中国人民公安大学侦查学院，北京 100038；2. 公安部物证鉴定中心，北京 100038；3. 中国人民公安大学公安管理学院，北京 100038）

摘要：硫化氢中毒的检验鉴定一直都是司法鉴定的难题，大量的硫化氢死亡案件由于检验方法的缺失导致无法确定死因。本文从硫化氢的物化特性、中毒机理及代谢、法医病理鉴定、毒物检验等角度进行综述，探究了色谱-质谱分析技术等不同硫化氢检验方法，总结出最为合适的硫化氢检验方法，并对硫化氢定量及现场检测进行展望，以期为其在司法鉴定领域的研究与应用提供参考与借鉴。

关键词：硫化氢；气相色谱；液相色谱；质谱；分光光度法

中图分类号：O65    文献标识码：A    文章编号：1000-0720（2023）10-1406-06

Research progress of detection techniques for hydrogen sulfide poisoning

ZHANG Zhen¹，ZHANG Yunfeng²，WU Xiaojun^*1，2，WANG Jifen¹，LU Pengwu³

1. School of Investigation，People’s Public Security University of China，Beijing 100038，China；2. Physical Evidence Identification Center of Ministry of Public Security，Beijing 100038，China；3. School of Public Security Management，People’s Public Security University of China，Beijing 100038，China）

Abstract：The detection and identification of hydrogen sulfide poisoning is always a difficult problem in judicial identification. In this paper，the physical and chemical characteristics of hydrogen sulfide，poisoning mechanism and metabolism，forensic pathological identification，poison test and other aspects were reviewed，the chromatography-mass spectrometry analysis technology and other different hydrogen sulfide test methods were explored，the most appropriate test method was summarized，quantitative and on-site detection of hydrogen sulfide were expected，aiming to provide reference for its research and application in the field of forensic expertise.

Keywords：hydrogen sulfide；gas chromatography；liquid chromatography；mass spectrometry；spectrophotometry

拉曼光谱技术在灵敏检测气味物质中的应用进展

文有青¹，李芷瑶¹，宁滢¹，王海霞^*1，2

（1. 天津中医药大学中药制药工程学院，天津 301617；2. 天津中医药大学省部共建组分中药国家重点实验室，天津 301617）

摘要：气味物质是食品和药品品质评价的重要指标之一。拉曼光谱技术，尤其是表面增强拉曼光谱技术，具有无损、高灵敏、检测速度快等优点，在气味物质灵敏检测方面具有突出优势。本文总结和梳理了气味物质化学结构与拉曼位移之间的关系，系统综述了拉曼光谱技术在甜、苦、酸、鲜和混合气味物质检测方面中的应用，并展望了该技术在气味物质检测领域的未来发展方向。

关键词：气味物质；表面增强拉曼光谱；快速检测；灵敏度

中图分类号：O657.37    文献标识码：A    文章编号：1000-0720（2023）10-1412-09

Advances of application of Raman spectroscopy for sensitive detection of odor substances

WEN Youqing¹，LI Zhiyao¹，NING Ying¹，WANG Haixia^*1，2

1. College of Pharmaceutical Engineering of Traditional Chinese Medicine，Tianjin University of Traditional Chinese Medicine，Tianjin 301617，China；2. State Key Laboratory of Component-based Chinese Medicine，Tianjin University of Traditional Chinese Medicine，Tianjin 301617，China）

Abstract：Odor is one of the important indexes for the quality evaluation of food and drug. Raman spectroscopy，especially surface enhanced Raman spectroscopy technique，with the advantages of non-destructive，high sensitivity and fast detection speed，has outstanding advantages in the sensitive detection of odor substances. This review summarizes the relationship between the chemical structure of odor and Raman shift，systematically summarizes the application of Raman spectroscopy technique in the detection of sweet，bitter，acid，fresh and mixed odor，and points out the future development direction of this technology in the field of odor detection.

Keywords：odor substances；surfaced enhanced Raman spectroscopy；rapid detection；sensitivity