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目的应用固相萃取-气相色谱/质谱联用技术,建立食用油中苯并(a)芘的检测方法。方法在试样中加入内标物,经KOH皂化后用正己烷萃取,用硅胶+硅藻土(SLH)固相萃取小柱净化后,经DB-5MS石英毛细管柱(30 m×0.25 mm×0.25μm)分离,用气质联用仪检测,选择离子模式测定。结果该方法检出限为0.3μg/kg,回收率为90.5%~98.9%,相对标准偏差为2.9%~3.5%。结论该方法简单、快速、净化效果好,灵敏度满足要求,能够快速准确地测定食用油中苯并(a)芘。
Objective To establish a method for the determination of benzo (a) pyrene in edible oil by solid-phase extraction coupled with gas chromatography / mass spectrometry. Methods The internal standard was added to the sample. After saponification with KOH, the sample was extracted with n-hexane, purified by silica gel + diatomite (SLH) solid-phase extraction cartridges and purified by DB-5MS quartz capillary column (30 m × 0.25 mm × 0.25μm) separation, detection by gas chromatography, the choice of ion mode determination. Results The detection limit was 0.3μg / kg, the recovery was 90.5% ~ 98.9% and the relative standard deviation was 2.9% ~ 3.5%. Conclusion The method is simple and rapid, the purification effect is good, the sensitivity meets the requirements, and the determination of benzo (a) pyrene in edible oil can be quickly and accurately performed.