卷烟主流烟气总粒相物、气相物和烟灰中吡虫啉等5种农药残留及其转移行为

Residues and transfer behaviors of five pesticides in cigarette mainstream smoke total particulate matter, gas phase and cigarette ash

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定主流烟气总粒相物、烟灰和气相物中吡虫啉、二甲戊灵、仲丁灵、甲霜灵和腈菌唑含量的方法。样品经乙腈提取,分散固相萃取后进行UPLC-MS/MS分析。各基质中5种农药的检出限为0.196~10.7 ng/cig,平均添加回收率为71%~118%,RSD为2.2%~12%。应用该方法研究了标准卷烟添加5种农药标准品和自然高残留样品中5种农药的烟气转移率。结果表明:标准卷烟添加5种农药标准品的主流烟气总粒相物中吡虫啉转移率相对较低(<7%),而其余4种农药转移率均大于30%;烟灰中未检出吡虫啉,其余4种农药转移率仅为0.1%~0.2%;此外,在主流烟气气相物中未检出目标农药。自然高残留卷烟样品主流烟气总粒相物中仅检出腈菌唑,且其转移率(2.6%~3.1%)远低于添加标准品的卷烟。

A new methods for the determination of imidacloprid, pendimethalin, butralin, metalaxyl, and myclobutanil residues in mainstream cigarette smoke total particulate matter （TPM）, cigarette ash and gas phase using ultra performance liquid chromatography-tandem mass spectrometry （UPLC- MS/MS） has been developed. Samples were extracted with acetonitrile, prepared by matrix dispersive solid phase extraction, and then analyzed by UPLC-MS/MS. The results showed that the LOD is from 0.196 to 10.7 ng/cig, the average recoveries ranged from 71%-118%, and the RSD ranged from 2.2%- 12%. This method was used to study the transfer behavior of five pesticides in standard cigarettes spiked with pesticide solutions and homemade cigarettes. The results showed that pendimethalin, butralin, metalaxyl, and myclobutanil were partly transferred to TPM （transfer ratio〉30%）, but the transfer ratio of imidacloprid in TPM was less than 7%. Few pesticides were transferred to cigarette ash （transfer ratio ： 0.1%-0.2%） except imidacloprid （transfer ratio ： 0）, and no pesticides transferred into gas phase of the mainstream smoke in standard spiked cigarettes. In homemade cigarettes, only little myclobutanil was transferred to TPM, and the transfer ratio （2.6%-3.1%） was much lower than that of the standard spiked cigarettes.