摘要
目的建立分散固相萃取结合高效液相色谱-串联质谱法(high performance liquid chromatographytandem mass spectrometry,HPLC-MS/MS)分析一次性筷子中5种杀菌剂的检测方法。方法一次性筷子试样经1%甲酸乙腈振荡提取,高速离心后取上层提取液,用酸性氧化铝粉末净化,经ZORBAX Eclipse Plus C18色谱柱分离后,采用多反应监测(multiple reaction monitoring,MRM)模式进行5种杀菌剂的测定,基质曲线外标法定量。结果5种杀菌剂在1~500ng/mL范围内呈现良好线性关系,相关系数为0.9967~0.9991,方法检出限为5.0μg/kg,定量限为10.0μg/kg。在5.0、10.0和100.0μg/kg 3个水平加标回收率为85.6%~106.8%,相对标准偏差为7.3%~9.9%(n=6)。结论该方法针对一次性筷子基质,采用酸性氧化铝粉末的净化方式,前处理方法简单、净化效果好,且灵敏度高、准确性好,适用于一次性筷子中常用杀菌剂的检测。
Objective To establish a method for determination of 5 types of fungicides in disposable chopsticks by dispersed solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The sample of disposable chopsticks was extracted by acetonitrile with 1%formic acid.The supernatant liquid was taken and purified with acidic alumina powder after high-speed centrifugation.Separated by ZORBAX Eclipse Plus C 18 chromatographic column,5 types of fungicides were finally determined by multiple reaction monitoring(MRM)mode.The calibration curve was set up by external standard calibration method.Results The linear relationship of 5 types of fungicides was strong in the range of 1-500 ng/mL.The correlation coefficient was 0.9967-0.9991,the limit of detection of the method was 5.0μg/kg and the limit of quantitation was 10.0μg/kg.The recoveries at the levels of 5.0,10.0 and 100.0μg/kg were 85.6%-106.8%,and the relative standard deviations ware 7.3%-9.9%(n=6).Conclusion Purified with acidic alumina powder,this method has a simple pretreatment,good purification effect,high sensitivity and excellent accuracy,which is especially applicable for the determination of common fungicides in disposable chopsticks.
作者
胡晓楠
张瑞华
郭文丽
张艾蕾
徐慧静
HU Xiao-Nan;ZHANG Rui-Hua;GUO Wen-Li;ZHANG Ai-Lei;XU Hui-Jing(Tianjin Institute for Food Safety Inspection Technology,Tianjin 300308,China)
出处
《食品安全质量检测学报》
CAS
2024年第3期183-189,共7页
Journal of Food Safety and Quality
基金
天津市市场监督管理委员会科技项目(2021-W21)。
关键词
杀菌剂
一次性筷子
高效液相色谱-串联质谱法
fungicide
disposable chopsticks
high performance liquid chromatography-tandem mass spectrometry
