基于通过型固相萃取-超高效液相色谱三重四级杆/复合线性离子阱质谱法测定调味酱中蟾蜍色胺  

Determination of bufotenine in sauces by ultra performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry with pass-through solid phase extraction

作　　者：孙文芳[1] 徐杰 朱峰[2] 杨雯 刘祥萍[1] 陈慧敏 SUN Wenfang;XU Jie;ZHU Feng;YANG Wen;LIU Xiangping;CHEN Huimin(Nanjing Center for Disease Control and Prevention,Jiangsu Nanjing 210003,China;Jiangsu Provincial Center for Disease Control and Prevention,Jiangsu Nanjing,210009,China;SCIEX Anylytical Intrument Trading Co.,Ltd,Shanghai 200335,China)

机构地区：[1]南京市疾病预防控制中心,江苏南京210003 [2]江苏省疾病预防控制中心,江苏南京210009 [3]SCIEX公司,上海200335

出　　处：《中国食品卫生杂志》2024年第12期1318-1324,共7页Chinese Journal of Food Hygiene

基　　金：南京市公共卫生检测重点实验室;南京市医学重点专科资助。

摘　　要：目的建立通过型固相萃取-超高效液相色谱三重四级杆/复合线性离子阱质谱法(UHPLC-QTRAP-MS/MS)测定调味酱中蟾蜍色胺含量的检测方法。方法样品匀浆后加入一定量的纯水和5%氨化乙腈超声提取。盐包盐析后,取上清液调节有机相比例及pH,通过PRiME HLB固相萃取小柱进行净化,净化液用纯水稀释离心后,UHPLC-QTRAP-MS/MS检测。同时结合线性离子阱采集的二级谱图与建立的标准谱库进行匹配分析。结果蟾蜍色胺在0.2~50.0 ng/mL浓度范围内线性关系良好,相关系数>0.999,方法检出限为0.4μg/kg,加标水平为5.0、50.0、200μg/kg时,回收率范围为99.5%~106.5%,相对标准偏差为1.9%~4.3%。结论该方法方便快捷,无须内标,抗干扰能力强,线性离子阱采集的二级质谱对样品进行二次辅助定性,可适用于应急事件调味酱中蟾蜍色胺含量的测定。Objective To establish a method for determination of bufotenine in sauces by ultra-high performance liquid chromatography-linear ion trap mass spectrometry(UHPLC-QTRAP-MS/MS)with pass-through solid phase extraction.Methods Samples were homogenized,extracted with water and ammoniated acetonitrile via ultrasonication.After salting out,the supernatant was taken to adjust the organic phase ratio and pH,then purified by PRiME HLB solid phase extraction column.After dilution and centrifugation with pure water,the purified liquid was detected by UHPLC-QRAPMS/MS.UHPLC-QTRAP-MS/MS technique automatically triggered an enhanced product ion scan(MRM-IDA-EPI)mode,collecting secondary mass spectra of suspected target compounds for comparison with standard spectra,thereby further identifying positive samples.Results Under optimized conditions,bufotenine can be effectively separated and showing good linearity in the concentration range from 0.2 to 50.0 ng/mL with correlation coefficients exceeding 0.999.The method’s detection limit was 0.4μg/kg,with an average recovery rate between 99.5%to 106.5%for spiked levels of 5.0,50.0 and 200μg/kg.A relative standard deviation from 1.9%to 4.3%.Conclusion It was a simple and rapid method,with secondary mass spectrometry collected by a linear ion trap,meeting the requirements for detecting bufotenine content in sauces.

关 键 词：蟾蜍色胺 调味酱 超高效液相色谱三重四级杆/复合线性离子阱质谱法 通过型固相萃取 

分 类 号：R155[医药卫生—营养与食品卫生学]