高效液相色谱-质谱联用法测定庆阳地产黄酒中环匹阿尼酸  

Determination of Cyclopiazonic Acid in Qingyang Local Huangjiu by HPLC-MS/MS

作　　者：徐娅茹 钱慜 陈德阳 孙国政 XU Yaru;QIAN Min;CHEN Deyang;SUN Guozheng(Qingyang Food Inspection and Testing Center,Qingyang 745000,China;Qingyang Center for Disease Control and Prevention,Qingyang 745000,China)

机构地区：[1]庆阳市食品检验检测中心,甘肃庆阳745000 [2]庆阳市疾病预防控制中心,甘肃庆阳745000

出　　处：《食品安全导刊》2022年第18期123-125,130,共4页China Food Safety Magazine

基　　金：甘肃省科技计划项目(20JR5RM628);甘肃省市场监督管理局科技计划项目(SSCJG-SP-201918)。

摘　　要：目的:采用高效液相色谱-三重四极杆质谱联用法测定庆阳地产黄酒中环匹阿尼酸含量。方法:样品经甲醇提取,过C色谱分析柱,以0.1%甲酸水溶液与甲醇为流动相梯度洗脱,采用高效液相色谱-质谱联用法正模式内标法测定分析,建立检测黄酒中环匹阿尼酸的分析方法。结果:液质联用法对黄酒中环匹阿尼酸最低检出限为0.6 ng·mL^(-1),定量限为2.0 ng·mL^(-1),精密度为0.71%;黄酒样品中环匹阿尼酸的加标回收率在99.7%~110.3%。结论:以甲醇为提取液,采用液质联用法可以对黄酒中环匹阿尼酸进行准确定性和定量,解决了液相色谱检测中常出现的假阳性问题,避免了对样品烦琐重复的提取过程,提高了大批量样品前处理的效率。Objective:To determine the content of cyclopiazonic acid in Qingyang local Huangjiu by HPLC-MS/MS.Method:The samples were extracted with methanol,analyzed with Cchromatographic column,eluted with 0.1% formic acid aqueous solution and methanol as mobile phase gradient,and analyzed with positive mode internal standard method by HPLC-MS/MS.An analytical method for the determination of cyclopiazonic acid in Huangjiu was established.Result:The minimum detection limit of detection of cyclopiazonic acid in Huangjiu was 0.6 ng·mL^(-1),the quantitative limit was 2.0 ng·mL^(-1),and the precision was 0.71%;the recoveries of cyclopiazonic acid in Huangjiu samples ranged from 99.7% to 110.3%.Conclusion:With methanol as the extraction solution,the method of HPLC-MS/MS can be used for accurate qualitative and quantitative determination of cyclopiazonic acid in Huangjiu,which solves the problem of false positive in liquid chromatography,avoids the tedious and repeated extraction process of samples,and improves the efficiency of mass sample pretreatment.

关 键 词：黄酒 环匹阿尼酸 超高效液相色谱-串联质谱法 庆阳 

分 类 号：O657.63[理学—分析化学] TS262.4[理学—化学]