纳米金表面增强拉曼光谱法快速定性定量检测3种非法添加抗感染药物  

Rapid Qualitative and Quantitative Detection of 3 Illegally Added Anti Infective Drugs by Nanogold Surface-Enhanced Raman Spectroscopy

作　　者：易路遥 蒋诗扬 仲雪 虞雪军 杨婷婷 洪燕 YI Luyao;JIANG Shiyang;ZHONG Xue;YU Xuejun;YANG Tingting;HONG Yan(Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiang Xi Institute for Drug Control,Nanchang 330029,China;ZLZJ(Suzhou)Biotech Co.,Ltd.,Suzhou 215000,China)

机构地区：[1]江西省药品检验检测研究院国家药品监督管理局中成药质量评价重点实验室江西省药品与医疗器械质量工程技术研究中心,南昌330029 [2]中朗正健(苏州)生物技术有限公司,苏州215000

出　　处：《理化检验（化学分册）》2023年第8期917-922,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江西省重点研发计划项目(20203BBGL73212);江西省药品监督管理局科技计划项目(2021KY08)。

摘　　要：以溶胶凝胶法制备的金纳米溶胶作基底,利用表面增强拉曼光谱法(SERS)对甲硝唑、依诺沙星、氟康唑等3种非法添加抗感染药物进行了定性定量研究。取1%(质量分数)氯金酸溶液950μL,加入60 mL水,于100℃剧烈搅拌至溶液沸腾,加入1%(质量分数)柠檬酸钠溶液0.6mL,静置20min至溶液颜色呈紫红色。冷却至室温,将所得的金纳米溶胶于4℃储存。取50μL标准溶液,加入450μL金纳米溶胶,利用拉曼光谱仪在100~3 000cm-1内进行检测。结果显示:3种抗感染药物的定性拉曼特征峰分别在1 180,1 264,1 364,1 550cm-1(甲硝唑),1 346,1 424cm-1(依诺沙星)和986,1 370cm-1(氟康唑)处,定量拉曼特征峰分别在1 364cm-1(甲硝唑),1 424cm-1(依诺沙星),986cm-1(氟康唑)处,其质量分数分别在0.500~10.000mg·kg^(-1)(甲硝唑)和2.000~20.000mg·kg^(-1)(依诺沙星和氟康唑)内和定量拉曼特征峰的峰面积呈线性关系,检出限(3.143s)为0.12~0.39mg·kg^(-1),回收率为88.5%~108%,测定值的相对标准偏差(n=7)为1.9%~5.3%。Using the nanogold sol prepared by the sol-gel method as the substrate,the qualitative and quantitative study of 3 illegally added anti infective drugs including metronidazole,enoxacin and fluconazole,was carried out by surface-enhanced Raman spectroscopy(SERS).An aliquot(950μL)of 1%(mass fraction)chloroauric acid solution was taken and mixed with 60 mL of water,and the mixture was vigorously stirred at 100℃ until the solution boiled,and 0.6 mL of 1%(mass fraction)sodium citrate solution was added.The above mixed solution was settled for 20 min until the solution color turned purple red,and cooled to room temperature.The resulting nanogold sol was stored at 4℃.The standard solution(50μL)was taken,and 450μL of nanogold sol was added.The mixture was detected within 100-3000 cm^(-1) using Raman spectrometer.It was shown that the qualitative Raman characteristic peaks of the 3 anti infective drugs were 1180,1264,1364,1550 cm^(-1) for metronidazole,1346,1424 cm^(-1) for enoxacin and 986,1370 cm^(-1) for fluconazole,respectively,with the quantitative Raman characteristic peaks of 1364 cm^(-1) for metronidazole,1424 cm^(-1) for enoxacin and 982 cm^(-1) for fluconazole.The linear relationships between values of the mass fraction and the peak area of the quantitative Raman characteristic peak of the 3 anti infective drugs were found in the ranges of 0.500-10.000 mg·kg^(-1)(metronidazole)and 2.000-20.000 mg·kg^(-1)(enoxacin and fluconazole),with detection limits(3.143s)in the range of 0.12-0.39 mg·kg^(-1),recoveries in the range of 88.5%-108%,and RSDs(n=7)of the determined values in the range of 1.9%-5.3%.

关 键 词：金纳米溶胶 表面增强拉曼光谱法(SERS) 甲硝唑 氟康唑 依诺沙星 定性检测 定量检测 

分 类 号：O657.37[理学—分析化学]