摘要
本文建立了一种自动顶空-固相微萃取结合气相色谱-串联质谱法(Automatic Headspace-Solid Phase Microextraction Combined with Gas Chromatography-Tandem Mass Spectrometry,Auto-SPME-GC-MS/MS)测定武都花椒中6种有机氯和5种拟除虫菊酯类农药的方法。采用自动顶空固相微萃取装置,自动在线完成样品加热、吸附、解吸、进样。通过改变不同萃取因素来探究萃取效率,确定最佳萃取纤维头、萃取试剂和萃取溶剂、盐用量、样品加热及振荡时间、样品吸附和解吸时间。结果显示,该方法的线性范围为0.01~1.00 ng·L^(-1),相关系数在0.998 7~0.999 9,呈现出良好的线性关系;方法检出限为0.005 ng·L^(-1);11种目标物的加标回收率在85.7%~104.4%,相对标准偏差在3.2%~9.6%。该方法准确度和精密度良好,可有效用于武都花椒中拟除虫菊酯类和有机氯农药的痕量分析。
This paper established a method for the determination of six organochlorines and five pyrethroid pesticides in Wudu pepper by automatic headspace-solid phase microextraction combined with gas chromatography-tandem mass spectrometry(Auto-SPME-GC-MS/MS).An automatic headspace solid-phase microextraction device is adopted to automatically complete sample heating,adsorption,desorption and injection online.The extraction efficiency was explored by changing different extraction factors to determine the optimal extraction fiber head,extraction reagents and extraction solvents,vortex time,salt concentration,sample heating and oscillation time,sample adsorption and desorption time.The results show that the linear range of this method is 0.01 ng·L-1 to 1.00 ng·L-1,and the correlation coefficient is between 0.9987 and 0.9999,presenting a good linear relationship;the detection limit of the method was 0.005 ng·L-1;the spiked recovery 190/现代食品XIANDAISHIPIN rates of the 11 target substances ranged from 85.7%%to 104.4%,and the relative standard deviations ranged from 3.2%to 9.6%.This method has good accuracy and precision and can be effectively used for trace analysis of pyrethroids and organochlorine pesticides in Wudu pepper.
作者
王小花
李波
尹娟娟
郭锌
周佳
WANG Xiaohua;LI Bo;YIN Juanjuan;Guo Xin;ZHOU Jia(Gansu Food Inspection and Research Institute,Lanzhou 730000,China;Gansu Engineering Research Center for Food Safety,Lanzhou 730000,China;Gansu Engineering Research Center for Nutrition and Safety Evaluation of Geographical Indication Products,Lanzhou 730000,China)
出处
《现代食品》
2025年第13期190-195,205,共7页
Modern Food
基金
甘肃省市场监督管理局科技计划项目(SSCJG-SP-B202204)
甘肃省科技计划项目自然科学基金(23JRRA1709)。
关键词
武都花椒
自动顶空-固相微萃取
气相色谱-串联质谱
有机氯
拟除虫菊酯
Wudu pepper
automatic headspace-solid phase microextraction
gas chromatography-tandem mass spectrometry
organochlorine pesticides
pyrethroids pesticides
