摘要
建立气相色谱-负化学源质谱法分析蔬菜中氟虫腈、氟虫腈砜、氟虫腈硫醚、氟甲腈4种化合物的测定方法,并进行方法的不确定度评定。样品用乙腈提取,经N-丙基乙二胺(Primary Secondary Amine, PSA)萃取净化,采用TR-PESTICIDE II色谱柱分离,基质标准溶液定量。氟虫腈及其代谢物在5~100 ng/mL范围内线性良好,方法检出限为0.002 mg/kg,定量限为0.020 mg/kg,在0.002, 0.010和0.020 mg/kg水平下加标回收率为86.9%~107.0%,相对标准偏差为0.6%~8.0%。评定结果表明,当生菜中氟虫腈、氟虫腈砜、氟虫腈硫醚、氟甲腈残留量为0.020 mg/kg时,扩展不确定度(k=2)分别为0.001 5, 0.001 4, 0.001 5和0.001 4 mg/kg,其残留量(k=2)分别为0.020±0.001 5, 0.020±0.001 4,0.020±0.001 5和0.020±0.001 4 mg/kg。该方法高效简单、灵敏度高,适合对蔬菜中氟虫腈及其代谢物进行分析,测定结果的不确定度来源主要是标准曲线的配制,可为蔬菜中分析氟虫腈及其代谢物测定量的准确性和可靠性提供技术补充。
tA method was developed for the determination of four pesticide residues fipronil,fipronil sulfone,fipronil sulfoxide and fipronil-desulfinyl in vegetables gas by gas chromatography-negative chemical ionization mass spectrometry,and the uncertainty was evaluated.The samples were extracted with acetonitrile,purified by Primary Secondary Amine(PSA),separated by Tr-PESTICIDE II column,and quantified by standard solution of matrix.The calibration curves showed good linearity in the range of 5-100 ng/mL for fipronil and its metabolites,the limit of detection was 0.002 mg/kg,and the limit of quantitative was 0.020 mg/kg.The recoveries ranged from 86.9%to 107.0%with the relative standard deviations ranged from 0.6%to 8.0%at the spiked levels of 0.002,0.010 and 0.020 mg/kg.The results showed that the expanded uncertainty(k=2)was 0.0015,0.0014,0.0015 and 0.0014 mg/kg,respectively,when the residues of fipronil,fipronil sulfone,fipronil sulfoxide and fipronildesulfinyl in vegetables were 0.020 mg/kg.Therefore,the residual amount(k=2)were expressed as 0.020±0.0015,0.020±0.0014,0.020±0.0015 and 0.020±0.0014 mg/kg.The main source of uncertainty was the calibration solution preparation.It provided an effective approach for raid and accurate determination of fipronil and its metabolite residues in vegetables,which could also provide the technical supplement for the accuracy and reliability of the determination of fipronil and its metabolite residues in vegetables by gas chromatography-negative chemical ionization mass spectrometry.
作者
林泽珊
黄松
赵金利
谭锦萍
黄穗东
刘佳
LIN Zeshan;HUANG Song;ZHAO Jinli;TAN Jinping;HUANG Suidong;LIU Jia(Guangzhou Institute for Food Inspection,Guangzhou 511400)
出处
《食品工业》
CAS
2023年第9期258-264,共7页
The Food Industry
基金
广州市市场监督管理局科技项目(222kj40)。
关键词
气相色谱-负化学源质谱法
氟虫腈及其代谢物
不确定度
蔬菜
外标法
s gas chromatography-negative chemical ionization mass spectrometry
fipronil and its metabolites
uncertainty
vegetables
external standard method
