为测定口含烟中甲醛、乙醛和巴豆醛,采用O-(2,3,4,5,6-五氟苄基)羟胺(PFBHA)衍生化GC-MS的方法,将口含烟经水萃取,与PFBHA反应生成相应的O-(2,3,4,5,6-五氟苄氧基)肟衍生产物,正己烷萃取后利用GC-MS分析正己烷相测定相应物质含量.甲醛、乙醛以D4-乙醛为内标,巴豆醛以D5-丁酮为内标,甲醛、乙醛检出限为0.010μg/g,巴豆醛检出限为0.001μg/g,各组分回收率为91.7%~104.1%,日内相对标准偏差≤5.3%,日间相对标准偏差≤9.6%.通过该方法测试的35个不同规格国外品牌口含烟,甲醛含量0.275~2.397μg/g,乙醛含量0.383~8.010μg/g,巴豆醛含量0.003~0.027μg/g.该方法前处理简单,灵敏度高,干扰少,结果准确,易于推广应用.%A derivatization gas chromatography-mass spectrometry (GC/MS) method with o-(2,3,4,5,6-pentafluorobenzyl)-hydroxylamine hydrochloride (PFBHA) was developed for the determination of formaldehyde, acetaldehyde and crotonaldehyde in tobacco products for oral use. Sample was extracted with water and part of aqueous extract was derivatizated with PFBHA. The PFBHA derivatives of carbonyls were extracted with hexane and analyzed by gas chromatography-mass spectrometry. The limits of detection ranged from 0.001-0.010 μg/g, with recoveries ranged from 91.7% to 104.1%. Results showed good inter-day repeatability (RSD≤9.6%) and intra-day repeatability (RSD≤ 5.3%). 35 main brand products sold in European and American markets were analyzed, formaldehyde (0.275-2.397 μg/g), acetaldehyde (0.383-8.010 μg/g) and crotonaldehyde (0.003-0.027 μg/g) were detected in all these tested products. This method was simple, accurate and suitable for the analysis of formaldehyde, acetaldehyde and crotonaldehyde in tobacco products for oral use.
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