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采用超高效液相色谱-串联质谱法测定烟草及卷烟烟气中常见多类型农药残留。

Determination of Commonly Used Multiclass Pesticide Residues in Tobacco and Cigarette Smoke by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry.

机构信息

Sichuan tobacco quality supervision and testing station, Chengdu, Sichuan 610041 P.R. China.

出版信息

J Chromatogr Sci. 2022 Jun 6;60(5):423-432. doi: 10.1093/chromsci/bmab113.

DOI:10.1093/chromsci/bmab113
PMID:34599330
Abstract

A novel method has been developed for the simultaneous determination of multiclass pesticide residues in tobacco and cigarette smoke, using a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) procedure and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Cigarette mainstream smoke particulate was collected on a Cambridge filter pad. Pesticide residues was extracted with an aqueous solution, back extracted into acetonitrile after freezing, purified by dispersive solid phase extraction with primary-secondary amine adsorbents and analyzed by UPLC-MS/MS. The obtained mean recoveries of 16 pesticides commonly used on tobacco at three fortification levels (5.9, 94.1 and 352.9 ng g-1) ranged from 69.3 to 115.9% with relative standard deviations between 2.4 and 11.3%. The limits of detection ranged from 0.14 to 13.28 ng g-1. Finally, the proposed method was applied to study the pesticide smoke transfer ratio in 2 cigarettes with pesticide standard spiked and 51 cigarettes with one or more pesticide residues. The transfer ratio of pesticides residue in tobacco into the smoke might be much less than that from artificially spiked tobacco (<25%) with spiking levels varied from 1.88 to 9.41 μg g-1. The transfer ratio of pesticide from artificially spiked tobacco into cigarette mainstream smoke was from 0.0 to 56.5%, and pesticide residues from tobacco into cigarette smoke were from 0.0 to 26.1% using the ISO smoking method (ISO 3308 2012).

摘要

一种新方法已经被开发用于同时测定烟草和香烟烟雾中的多类农药残留,使用改良的 QuEChERS(快速、简单、便宜、有效、坚固和安全)方法和超高效液相色谱-串联质谱法(UPLC-MS/MS)。香烟主流烟雾颗粒收集在剑桥滤垫上。用水溶液提取农药残留,冷冻后用乙腈反萃取,用初级-次级胺吸附剂分散固相萃取净化,然后用 UPLC-MS/MS 分析。在三个加标水平(5.9、94.1 和 352.9ng/g-1)下,16 种常用烟草农药的平均回收率为 69.3%至 115.9%,相对标准偏差在 2.4%至 11.3%之间。检测限范围为 0.14 至 13.28ng/g-1。最后,该方法应用于研究 2 支有农药标准添加香烟和 51 支有 1 种或多种农药残留香烟中的农药烟雾转移比。从人工添加烟草中(1.88 至 9.41μg/g-1)进入烟雾的农药残留转移比可能远小于从人工添加烟草中(<25%)进入烟雾的转移比。从人工添加烟草到香烟主流烟雾的农药转移比为 0.0 至 56.5%,从烟草到香烟烟雾的农药残留转移比为 0.0 至 26.1%,使用 ISO 吸烟方法(ISO 3308 2012)。

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