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

中文关键词:  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

英文关键词:gas chromatography-mass spectrometry  complex matrix  tea  paprika  vinclozolin  3,5-dichloroaniline

中文摘要:

      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。

英文摘要:

      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.