液相色谱-串联质谱法测定葡萄中链霉素和双氢链霉素  

Determination of streptomycin and dihydrostreptomycin in grapes by liquid chromatography-tandem mass spectrometry

作　　者：刘真真[1] 齐沛沛[1] 何付香 汪志威[1] 狄珊珊 徐浩[1] 赵慧宇[1] 王强[1] 王新全[1] LIU Zhenzhen;QI Peipei;HE Fuxiang;WANG Zhiwei;DI Shanshan;XU Hao;ZHAO Huiyu;WANG Qiang;WANG Xinquan(Institute of Quality and Standard of Agro-Products, Zhejiang Academy of Agricultural Sciences, State Key Laboratory for Managing Biotic and Chemical Theats to the Quality and Safety of Agro-Products, Hangzhou 310021, China)

机构地区：[1]浙江省农业科学院农产品质量标准研究所,农产品质量安全危害因子与风险防控国家重点实验室,浙江杭州310021

出　　处：《色谱》2020年第12期1396-1401,共6页Chinese Journal of Chromatography

基　　金：现代农业产业技术体系建设专项(CARS-29).

摘　　要：研究系统地优化了样品前处理过程及仪器分析中影响链霉素和双氢链霉素残留分析准确度与响应灵敏度的各主要因素,建立了葡萄中链霉素和双氢链霉素残留的快速精准定量分析方法。葡萄样品经磷酸溶液(pH=2)超声提取、Oasis HLB单固相萃取柱富集净化后,采用Waters HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离,柱温35℃,进样量2μL,以0.1%甲酸水溶液-甲醇溶液(60∶40,v/v)为流动相进行等度洗脱,在正离子、电喷雾电离源多反应监测模式下测定,外标法定量。链霉素和双氢链霉素在2~400μg/L质量浓度范围内线性关系良好,相关系数(R2)分别为0.9991和0.9997;在5、10、20和40μg/kg 4个添加水平下的平均回收率为76.8%~91.9%,相对标准偏差为0.4%~10.2%;链霉素和双氢链霉素的检出限(LOD)为1μg/L,定量限(LOQ)为5μg/kg。为验证该方法的适用性,将方法适用于无籽红提、新郁葡萄、夏黑葡萄等实际样品中进行添加回收实验,链霉素和双氢链霉素的平均回收率分别为77.2%~83.9%和70.8%~78.9%,RSD为3.0%~15.6%。该法的准确度和精密度均符合葡萄中链霉素和双氢链霉素分析要求,且操作简便、准确,灵敏度高,适用于葡萄中链霉素和双氢链霉素残留量的检测分析。Streptomycin(STR)and dihydrostreptomycin(DSTR)are two of the most common aminoglycoside antibiotics used in veterinary medicine.STR is produced by some streptomyces griseus strains,and DSTR is a derivative of STR.In recent years,STR has been widely used in grapes to induce denuclearization.However,high levels of STR may have adverse effects like serious ototoxicity and nephrotoxicity.Therefore,to ensure the quality of grapes and the health of consumers,the regulation of STR and DSTR levels in grapes is required.An analytical method was developed for the identification and quantification of STR and DSTR in grapes by liquid chromatography-tandem mass spectrometry(LC-MS/MS).STR and DSTR are highly polar compounds due to the presence of various amino and hydroxyl groups in their structure.The determination of STR and DSTR poses a considerable analytical challenge,both during sample preparation and instrument analysis.In this study,the main factors governing the response,recovery,and sensitivity of these compounds,such as the type of chromatographic column,the type and proportion of the mobile phase and extraction solvent,the dosage of sodium 1-hexane sulfonate solution,and elution solvent and its volume,were investigated during sample pretreatment and instrument analysis.The STR and DSTR residues in the grape sample were extracted by ultrasonication with a phosphoric acid solution(pH 2),and cleanup and enrichment was performed using an Oasis HLB solid phase column.The analysis was performed using a UPLC Waters HSS T3 column(100 mm×2.1 mm,1.8μm)at the column temperature of 35℃.The injection volume was 2μL.The mobile phase consisted of 0.1%formic acid aqueous solution and methanol with a volume ratio of 60∶40.ESI-MS/MS was operated in multiple reaction monitoring(MRM)mode.External standard calibration curves were used for quantification.Based on the optimized method,both analytes displayed good linearity between 2 and 400μg/L.The correlation coefficients were 0.9991-0.9997.Recoveries in spiked blank grape sampl

关 键 词：液相色谱-串联质谱 固相萃取 链霉素 双氢链霉素 葡萄 

分 类 号：O658[理学—分析化学]