多壁碳纳米管/N-丙基乙二胺混合吸附-超高效液相色谱-串联质谱法测定普洱茶中3种手性杀菌剂农药残留  

Determination of 3 chiral fungicide pesticide residues in Pu-erh tea by multiwalled carbon nanotubes/primary secondary amine mixed adsorption-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：蒋明明 曾小娟 宋红坤 林涛[2] 王继良 刘宏程[2] JIANG Ming-Ming;ZENG Xiao-Juan;SONG Hong-Kun;LIN Tao;WANG Ji-Liang;LIU Hong-Cheng(School of Pharmacy,Kunming Medical University,Kunming 650500,China;Institute of Quality Standard and Testing Technology,Yunnan Academy of Agricultural Sciences,Kunming 650223,China)

机构地区：[1]昆明医科大学药学院,昆明650500 [2]云南省农业科学院质量标准与检测技术研究所,昆明650223

出　　处：《食品安全质量检测学报》2020年第6期1702-1708,共7页Journal of Food Safety and Quality

基　　金：国家自然科学基金项目(31760490)。

摘　　要：目的建立基于手性柱/超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定普洱茶生茶和熟茶中3种手性农药(三唑酮、苯霜灵、丙环唑)对映体的分析方法。方法样品采用乙腈提取,氨基化多壁碳纳米管(aminated multi-walled carbon nanotubes,MWCNTs-NH2)和N-丙基乙二胺(primary secondary amine,PSA)混合吸附剂净化,经手性色谱柱Chiralpak-IG拆分,超高效液相-串联质谱法检测,基质外标法定量。结果3种农药外消旋体在0.005~1.0 mg/L范围内均呈良好线性关系,定量限(limits of quantification,LOQ)为0.005~0.01 mg/kg。在3种手性农药单个对映体含量为0.1、0.01、0.0025 mg/kg加标水平下平均回收率为70.1%~110.6%,相对标准偏差(relative standard deviation,RSD)(n=6)为1.2%~13.5%。结论该方法准确、简单、灵敏,可以满足普洱茶中3种手性农药对映体残留的检测要求。Objective To establish a method for the determination of the enantiomers of 3 kinds of chiral pesticides(triadimefon,benalaxyl,propiconazole)in Pu-erh raw tea and ripe tea by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with chiral column.Methods The sample was extracted with acetonitrile,then purified with aminated multi-walled carbon nanotubes and primary secondary amine.After separated with a Chiralpak-IG chiral column,the extract was detected by UPLC-MS/MS and quantified by matrix external standard method.Results The 3 kinds of racemates of pesticides showed a good linear relationship in the range of 0.005 to 1.0 mg/L,the limit of quantification was 0.005-0.01 mg/kg.The recoveries at the single enantiomeric content of 3 spiked levels of 0.1,0.01,0.0025 mg/kg were in the range of 70.1%-110.6%with relative standard deviations(n=6)of 1.2%-13.5%.Conclusion This method is accurate,simple and sensitive,and can meet the requirements for the detection of 3 kinds of enantiomeric residues of chiral pesticides in Pu-erh tea.

关 键 词：超高效液相-串联质谱法 手性拆分 对映体 普洱茶 

分 类 号：O657.63[理学—分析化学] TS272.7[理学—化学]