ＱｕＥＣｈＥＲＳ－气相色谱串联质谱法检测诺丽酵素原液中12种农药残留
时间：2021-02-08 08:02:09 来源：雅意学习网 本文已影响 人 
摘要：建立了QuEChERS净化结合气相色谱串联质谱测定诺丽酵素原液中12种农药残留的方法。样品采用乙腈溶液提取，提取液中加入无水硫酸镁、氯化钠、柠檬酸钠、柠檬酸氢二钠脱水和缓冲，振荡分层后吸取上层清液，再经PSA净化离心后上机。结果表明，50 mg PSA能够满足方法的净化要求，12种农药均采用外标法定量，基质标准溶液在0.005～0.960 mg/L线性良好;在0.012、0.080、0.400 mg/kg 3个添加水平下回收率为84.2%～113.0%，RSD均小于15%，大部分农药定量限为0.012 mg/kg。该方法前处理简单快速，准确度和精密度符合检测要求，可满足诺丽酵素原液中的乙烯菌核利、腐霉利、联苯菊酯等12种农药残留的同时检测。
关键词：诺丽酵素原液;农药;QuEChERS;气相色谱串联质谱
中图分类号：O657.7+1 文献标识码：A
文章编号：0439-8114（2019）01-0096-04
DOI：10.14088/j.cnki.issn0439-8114.2019.01.023 开放科学（资源服务）标识码（OSID）：
Simultaneous Determination of Fermentation Broth of Morinda Citrifolia using QuEChERS-Gas Chromatography-tandem Mass Spectrometry
WU Nan-cun1，2，ZHANG Qun1，2，LIU Chun-hua1，2，MA Chen1，2，WU Xue-jin1，2
（1. Analysis and Testing Center，Chinese Academy of Tropical Agricultural Sciences，Haikou 571101，China;
2.Hainan Key Laboratory for Quality and Safety of Tropical Fruits and Vegetables，Haikou 571101，China）
Abstract： A method has been developed for the simultaneous determination of 12 pesticides residues in fermentation broth of Morinda citrifolia using QuEChERS-gas chromatography-tandem mass spectrometry. The residue of 12 pesticides were extracted from samples by acetonitrile，then the extracting solution was cleaned up with PSA. Finally，the pesticides was analysed by gas chromatography-mass spectrometry under MRM mode via electrospray ionization.All pesticides were quantified by external standard method. The matrix calibration curves of the pesticides were linear in the range of 0.005～0.960 mg/L. The average recoveries of target compounds at three spiked concentration levels of 0.012，0.08，0.40 mg/kg were in the range of 84.2%～113.0%， RSD were less than 15%， the limit of quantification of most pesticides were 0.012 mg/kg. The results demonstrated the method is simple， fast aaccurated and can be used for analysis of the multiclass of pesticide residues in fermentation broth of morinda citrifolia.
Key words： Morinda citrifolia; pesticides; QuEChERS; gas chromatography-tandem mass spectrometry
諾丽（Noni）是茜草科巴戟天属的一种植物，学名海滨木巴戟（Morinda citrifolia Linn.），生长于热带和亚热带地区，是玻利尼西亚土著民有名的药用植物。研究表明诺丽果实含有黄酮化合物、环烯醚萜类化合物、氨基酸等对人体有益的成分[1-3]。国内由诺丽果开发的产品越来越多，诺丽酵素由诺丽果发酵而成，是诺丽产品中最受欢迎的品种。目前中国海南、西沙、云南和台湾等地均有诺丽的种植，海南和云南的种植已有一定的规模[4，5]，市场上也有诺丽产品中农药残留的检测需求。
果树种植中常用有机氯和拟除虫菊酯类农药，这些农药目前的检测方法多为气相色谱、气相质谱法[6-8]。其中气相串联质谱法抗干扰能力强，且能够更准确的定量和定性，对实现多种农药的同时测定更有帮助。本研究以气相色谱-串联质谱法为检测手段，采用乙二胺基-N-丙基（PSA）为净化吸附剂，优化了各农药的碰撞能量等质谱参数，开发了一种简单高效的诺丽酵素原液中乙烯菌核利、腐霉利、联苯菊酯等12种农药残留的检测方法。
