冷冻除脂-气相色谱-串联质谱法检测食用植物油中30 种多环芳烃

doi:10.7506/spkx1002-6630-201808044

食品科学 ›› 2018, Vol. 39 ›› Issue (8): 282-287.doi: 10.7506/spkx1002-6630-201808044

冷冻除脂-气相色谱-串联质谱法检测食用植物油中30 种多环芳烃

王国庆，王宗义*，程明捷，翟孟婷，马蒙蒙，黄漫青

（北京农学院食品科学与工程学院，食品质量安全北京实验室，农产品有害微生物及农残安全检测与控制北京市重点实验室，北京 102206）

出版日期:2018-04-25 发布日期:2018-04-17
基金资助:
北京市教委食品质量与安全北京实验室建设专项（PXM2017-014207-000038）；北京农学院实验技术体系基金项目（1086716287）

Determination of 30 Polycyclic Aromatic Hydrocarbons in Edible Vegetable Oils by Freeze Defatting Combined with Gas Chromatography-Tandem Mass Spectrometry

Wang Guoqing, Wang Zongyi*, Cheng Mingjie, Zhai Mengting, Ma Mengmeng, Huang Manqing

(Beijing Laboratory of Food Quality and Safety, Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides, College of Food Sciences and Engineering, Beijing University of Agriculture, Beijing 102206, China)

Online:2018-04-25 Published:2018-04-17

摘要/Abstract

摘要： 建立冷冻除脂--气相色谱-串联质谱检测食用植物油中30?种多环芳烃（polycyclic aromatic hydrocarbons，PAH）的方法。选用6?种氘标记PAH为内标，样品经乙腈--丙酮溶液（4∶1，V/V）于离心管中涡旋提取，10?000?r/min离心5?min，－80?℃对油脂冷冻固化，倾出提取液，再经减压浓缩和氮气吹干，以二氯甲烷复溶，气相色谱--串联质谱多反应监测方式进行检测。结果表明，在相应质量浓度范围内30?种PAH均有良好线性（R2＞0.998），检出限为0.10～1.83?μg/kg，定量限为0.35～6.11?μg/kg，在5、20?μg/kg和50?μg/kg添加水平下的回收率为67.77%～119.28%，相对标准偏差为1.18%～12.47%。采用本方法对市售11?类38?个食用植物油样品的检测显示，萘、1-甲基萘、2--甲基萘、联苯、2,6--二甲基萘、苊烯、苊、2,3,6--三甲基萘、芴、二苯并噻吩、菲、蒽、1-甲基菲、荧蒽、芘、环戊烯[c,d]芘、苯并[a]蒽、屈、苯并[b]荧蒽、苯并[k]荧蒽、苯并[e]芘和苯并[a]芘的检出率均为100%；5--甲基屈、苝、茚并[1,2,3--c,d]芘、二苯并[a,h]蒽、苯并[g,h,i]苝和二苯并[a,l]芘的检出率分别为86.84%、63.16%、81.58%、21.05%、81.58%和26.32%；二苯并[a,e]芘和二苯并[a,h]芘未检出；PAH总量为92.56～905.16?μg/kg，其中苯并[a]芘含量为1.94～7.40?μg/kg，依据食品安全标准限量，PAH处于较安全水平。

关键词: 食用植物油, 冷冻除脂, 多环芳烃, 气相色谱-串联质谱

Abstract: A new method was developed for the determination of 30 polycyclic aromatic hydrocarbons (PAHs) in edible vegetable oils by gas chromatography-tandem mass spectrometry (GC-MS/MS) after freeze defatting. Six deuterium labeled PAHs were used as internal standards. Samples were extracted with acetonitrile-acetone (4:1, V/V) by vortex mixing in a centrifuge tube followed by 5 min centrifugation at 10 000 r/min and freezing at ?80 ℃ for fat solidification. The extract was evaporated in a rotary vacuum evaporator and blown to dryness under nitrogen. The residue was re-dissolved in dichloromethane, and detected using GC-MS/MS in the multiple reaction monitoring mode. The calibration curves for all the analytes showed good linearity (R2 > 0.998) in their respective concentration ranges. The limits of detection (LODs) and limits of quantitation (LOQs) for 30 PAHs were in the ranges of 0.10–1.83 and 0.35–6.11 μg/kg, respectively. The recoveries varied from 67.77% to 119.28% with relative standard deviation (RSDs) of 1.18%–12.47% (n = 6) at spiked levels of 5, 20 and 50 μg/kg. The levels of 30 PAHs in 38 commercial edible vegetable oil samples from 11 different species were investigated using the GC-MS/MS method. The results showed that naphthalene, 2-methylnaphthalene, 1-methylnaphthalene, biphenyl, 2,6-bimethylnaphthalene, acenaphthylene, acenaphthene, 2,3,6-trimethylnaphthalene, fluorene, dibenzothiophene, phenanthrene, anthracene, 1-methylphenanthrene, fluoranthene, pyrene, cyclopenta[c,d]pyrene, benzo[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[e]pyrene and benzo[a]pyrene were detected in all samples; the detection rates of 5-methylchrysene, perylene, indeno[1,2,3-c,d]pyrene, dibenz[a,h]anthrancene, benzo[g,h,i]perylene and dibenzo[a,l]pyrene were 86.84%, 63.16%, 81.58%, 21.05%, 81.58% and 26.32%, respectively; neither dibenzo[a,e]pyrene nor dibenzo[a,h]pyrene were detected in any of the samples. The total concentrations of 30 PAHs ranged from 92.56 to 905.16 μg/kg, and BAP varied from 1.94 to 7.40 μg/kg, which were at safe levels according to the limit standard.

Key words: edible vegetable oil, freeze defatting, polycyclic aromatic hydrocarbons, gas chromatography-tandem mass spectrometry (GC-MS/MS)

中图分类号:

TS202.3

王国庆，王宗义，程明捷，翟孟婷，马蒙蒙，黄漫青. 冷冻除脂-气相色谱-串联质谱法检测食用植物油中30 种多环芳烃[J]. 食品科学, 2018, 39(8): 282-287.

Wang Guoqing, Wang Zongyi, Cheng Mingjie, Zhai Mengting, Ma Mengmeng, Huang Manqing. Determination of 30 Polycyclic Aromatic Hydrocarbons in Edible Vegetable Oils by Freeze Defatting Combined with Gas Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2018, 39(8): 282-287.

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冷冻除脂-气相色谱-串联质谱法检测食用植物油中30 种多环芳烃

Determination of 30 Polycyclic Aromatic Hydrocarbons in Edible Vegetable Oils by Freeze Defatting Combined with Gas Chromatography-Tandem Mass Spectrometry

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