气相色谱-质谱联用法测定茶叶和辣椒粉中的乙烯菌核利及其代谢物3,5-二氯苯胺残留量  

Determination of vinclozolin and its metabolite 3,5-dichloroaniline residues in tea and paprika by gas chromatography-mass spectrometry

作　　者：侯颖烨 李菊 曾广丰 王璐 谢建军 HOU Ying-Ye;LI Ju;ZENG Guang-Feng;WANG Lu;XIE Jian-Jun(Technology Center of Guangzhou Customs,Guangzhou 510623,China)

机构地区：[1]广州海关技术中心,广州510623

出　　处：《食品安全质量检测学报》2021年第10期4155-4160,共6页Journal of Food Safety and Quality

基　　金：海关总署技术规范研制项目(2019B112)。

摘　　要：目的建立气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)测定茶叶和辣椒粉中的乙烯菌核利及其代谢物3,5-二氯苯胺残留量的分析方法。方法茶叶和辣椒粉样品用乙腈振荡提取,提取液过复杂基质(multiplug filtration clean-up,m-PFC)快速滤过型固相萃取(solid phase extraction,SPE)柱净化,滤液氮吹至近干,用乙酸乙酯定容后用GC-MS进行测定,外标法定量。结果乙烯菌核利及其代谢物3,5-二氯苯胺的质量浓度在20~200 ng/mL范围内与其峰面积呈良好的线性关系。乙烯菌核利和3,5-二氯苯胺的定量限(limit of quantification,LOQ)在茶叶中为0.33 mg/kg,在辣椒粉中为0.07 mg/kg,加标回收率为83.3%~93.5%,相对标准偏差(relative standard deviation,RSD)为1.12%~8.11%。结论该方法操作简单、准确,可应用于茶叶和辣椒粉中的乙烯菌核利及其代谢物3,5-二氯苯胺残留量的检测。Objective To establish a method for the determination of vinclozolin and 3,5-dichloroaniline residues in tea and paprika by gas chromatography-mass spectrometry(GC-MS).Methods Samples were extracted by vibration ultrasonic with acetonitrile,then the extracts were purified by multiplug filtration clean-up solid phase extraction cartridges.The filtrate was evaporated to dryness by nitrogen evaporator and the residues were diluted with ethyl acetate,which was used for GC-MS analysis,and quantified by external standard method.Results Linear relationship between values of peak area and mass concentration of vinclozolin and 3,5-dichloroaniline were good in the range of 20-200 ng/mL.The limits of quantification(LOQ)of vinclozolin and 3,5-dichloroaniline in tea and paprika were 0.33 mg/kg and 0.07 mg/kg,the recoveries rate were 83.3%-93.5%and relative standard deviations were 1.12%-8.11%.Conclusion This method is accurate and easy,and it can be used for the determination of vinclozolin and 3,5-dichloroaniline residues in tea and paprika.

关 键 词：气相色谱-质谱联用法 复杂基质 茶叶 辣椒粉 乙烯菌核利 3 5-二氯苯胺 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]