摘要
目的:建立超高效液相色谱-串联质谱法测定蜂蜜中链霉素(Streptomycin,SM)和双氢链霉素(Dihydrostreptomycin,DHSM)的残留量。方法:试样经2%三氯乙酸、10 mmol·L^(-1)乙酸铵、0.4 mmol·L^(-1)乙二胺四乙酸二钠盐水合物和0.5%NaCl溶液提取后过Oasis HLB柱净化,并以10%甲酸-5%异丙醇-水溶液洗脱,过滤膜后采用超高效液相色谱-串联质谱法进行分析。采用SIELC Obelisc R色谱柱,以乙腈-0.5%甲酸溶液(pH=2.5)为流动相进行梯度洗脱,多反应监测模式测定,外标法定量。结果:SM和DHSM在2.5~100.0 ng·mL^(-1)呈现良好的线性关系,检出限为2μg·kg^(-1)、定量限为5μg·kg^(-1);平均加标回收率(n=6)为90.0%~97.5%,相对标准偏差(n=6)为0.4%~4.2%。结论:该方法满足链霉素与双氢链霉素的检测要求,灵敏度高、操作简单,适用于大批量蜂蜜样品中链霉素与双氢链霉素的检测。
Objective:To establish an ultra-high performance liquid chromatography tandem mass spectrometry method for the determination of residual levels of streptomycin(SM)and dihydrostreptomycin(DHSM)in honey.Method:The sample was extracted with 2%trichloroacetic acid,10 mmol·L^(-1) ammonium acetate,0.4 mmol·L^(-1) ethylenediaminetetraacetic acid disodium salt hydrate,and 0.5%NaCl solution.It was purified using an Oasis HLB column and eluted with a 10%formic acid-5%isopropanol aqueous solution.The membrane was filtered and analyzed using ultra-high performance liquid chromatography tandem mass spectrometry.Using SIELC Obelisk R chromatography column,gradient elution was performed with acetonitrile 0.5%formic acid solution(pH=2.5)as the mobile phase.Multiple reaction monitoring mode was used for determination,and external standard method was used for quantification.Result:SM and DHSM showed a good linear relationship between 2.5~100.0 ng·mL^(-1),with a detection limit of 2μg·kg^(-1) and a quantification limit of 5μg·kg^(-1);the average recovery rate(n=6)is 90.0%to 97.5%,and the relative standard deviation(n=6)is 0.4%to 4.2%.Conclusion:This method meets the detection requirements of streptomycin and dihydrostreptomycin,with high sensitivity and simple operation,and is suitable for the detection of streptomycin and dihydrostreptomycin in large quantities of honey samples.
作者
王岩
刘璐
贾祥坤
黄婕
秦钲懿
靳志敏
WANG Yan;LIU Lu;JIA Xiangkun;HUANG Jie;QIN Zhengyi;JIN Zhimin(Inner Mongolia Autonomous Region Administration of Market Supervision Evaluation and Inspection Center,Hohhot 010000,China)
出处
《食品安全导刊》
2025年第15期72-76,共5页
China Food Safety Magazine
关键词
超高效液相色谱-串联质谱法
链霉素
双氢链霉素
ultra high performance liquid chromatography-tandem mass spectrometry
streptomycin
dihydrostreptomycin
作者简介
王岩(1989-),男,内蒙古呼和浩特人,硕士,高级工程师。研究方向:食品工程。;通信作者:靳志敏(1985-),女,内蒙古呼和浩特人,博士,正高级工程师。研究方向:食品科学。E-mail:jzm201009@126.com。
