高效液相色谱串联质谱法测定动物源性食品中苯佐卡因、利多卡因  

Determination of benzocaine and lidocaine residues in animal derived foods by HPLC-MS/MS

作　　者：陆静 申甜甜 焦艳娜 梁香 朱绍华 刘紫涵 夏雨桑 付善良 成婧 LU Jing;SHEN Tiantian;JIAO Yanna;LIANG Xiang;ZHU Shaohua;LIU Zihan;Xia Yusang;FU Shanliang;CHENG Jing(Technology Center of Changsha Customs,Hunan Key Laboratory of Food Safety Science&Technology,Changsha 410004,China)

机构地区：[1]长沙海关技术中心,食品安全科学技术湖南省重点实验室,长沙410004

出　　处：《化学分析计量》2023年第5期56-62,67,共8页Chemical Analysis And Meterage

基　　金：海关总署科技计划项目(2021HK202)、长沙海关科技微创新项目(2021)。

摘　　要：建立高效液相色谱串联质谱法检测动物源性食品中的苯佐卡因、利多卡因残留量的分析方法。称取粉碎后的样品5.0 g,置于50 mL离心管中,加入1 g NaCl,10 mL乙腈,振荡提取20 min后,以4500 r/min转速离心5 min,取上清液6 mL,分别加入乙二胺-N-丙基硅烷(pPSA)50 mg、C1850 mg,然后在涡旋仪上涡旋1 min,以4500 r/min转速离心5 min,然后取0.5 mL上清液与0.5 mL复溶液[0.1%甲酸-乙腈(体积比为80∶20)混合液]混合,过0.22μm滤膜,供高效液相色谱串联质谱法测定。以0.1%乙酸-乙腈为流动相,C18柱为色谱柱,多反应监测模式分析,色谱峰面积外标法定量。苯佐卡因和利多卡因在0.1~50.0μg/L的质量浓度范围内线性关系良好,相关系数均大于0.999,检出限分别为0.2、0.1μg/kg,定量限分别为0.7、0.5μg/kg,回收率分别为85.0%~100.6%、87.7%~99.8%,5次测定结果的相对标准偏差分别为0.3%~3.5%、1.8%~3.6%。该方法可以满足动物源性食品中苯佐卡因、利多卡因同时检测的需要。A method was established for the determination of benzocaine and lidocaine in animal derived foods by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).5.00 g of sample was put into a 50 mL centrifuge tube with 1 g sodium chloride,then 10 mL acetonitrile was added as extraction solvent,and shaken for 20 min.The sample tubes centrifuged at 4500 r/min for 5 min.Then 50 mg octadecyl trimethoxysilane powder(C18)and 50 mg n-propyl ethylenediamine powder(PSA)were added into 6 mL of the supernatant,the mixture was mixed well by vortex for 1 min.The sample tubes centrifuged at 5500 r/min for 5 min,then mixed 0.5 mL of supernatant with 0.5 mL of complex solution[0.1%formic acid-acetonitrile(80∶20,volume ratio)]and analyzed by HPLC-MS/MS after filtered through a 0.22μm membrane.Gradient elution was performed by using acetonitrile and 0.1%acetic acid.The mass spectrometric acquisition was carried out by means of multiple reaction monitoring(MRM)after separated by C18 column.Good linearity was obtained in the range of 0.1-50.0μg/L for benzocaine and lidocaine,the correlation coefficient were more than 0.999.The limits of detection(LOD)for benzocaine and lidocaine were 0.2,0.1μg/kg,respectively.The limits of quantitation(LOQ)for benzocaine and lidocaine were 0.7,0.5μg/kg,respectively.The recoveries were 85.0%-100.6%and 87.7%-99.8%,respectively.The relative standard deviations of the five determinations were 0.3%-3.5%and 1.8%-3.6%,respectively.This method is suitable for the determination of benzocaine and lidocaine in animal derived foods.

关 键 词：高效液相色谱串联质谱法 苯佐卡因 利多卡因 动物源性食品 

分 类 号：O657.63[理学—分析化学]