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

摘要/Abstract

摘要： 建立了冷冻除脂-气相色谱串联质谱(GC-MS/MS)检测食用植物油中30种多环芳烃(PAH)的新方法。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，离心分离，-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，在相应浓度范围内30种PAH均有良好线性(R2≥0.999)，检出限为0.10~1.83 μg/kg，定量限为0.35~6.11 μg/kg，在5、20和50μg/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(NAP)、1-甲基萘(1-MNAP)、2-甲基萘(2-MNAP)、联苯(BIPH)、2,6-二甲基萘(DMNAP)、苊烯(ACY)、苊(ACE)、2,3,6-三甲基萘(TMNAP)、芴(FLU)、二苯并噻吩(DBTP)、菲(PHE)、蒽(ANT)、1-甲基菲(1-MPHE)、荧蒽(FLUR)、芘(PYR)、环戊烯[c,d]芘(CPP)、苯并[a]蒽(BAA)、屈(CHR)、苯并[b]荧蒽(BBF)、苯并[k]荧蒽(BKF)、苯并[e]芘(BEP)和苯并[a]芘(BAP)的检出率均为100%；5-甲基屈(5-MCHR)、苝(PER)、茚并[1,2,3-c,d]芘(ICDP)、二苯并[a,h]蒽(DBAHA)、苯并[g,h,i]苝(BGHIP)和二苯并[a,l]芘(DBALP)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(DBAEP)和二苯并[a,h]芘(DBAHP)未检出；PAH总量为92.56~905.16 μg/kg，其中BAP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) with removing fat through freezing. With six kinds of deuterium labeled PAHs as internal standards, the edible vegetable oil sample was extracted with acetonitrile-acetone (4+1, V/V) by vortex mixing in centrifuge tube, then the extract solution was frozen to make the fat solidification at -80℃ after centrifugation adequately and was separated from the solid fat at bottom of the centrifuge tube by transferring the solution to the evaporating bottle. Next, the extract solution was evaporated to dryness by a rotary vacuum evaporator and nitrogen flow in turn. The residue was re-dissolved in dichloromethane, and the detection were performed using GC-MS/MS in MRM mode. All analytes showed good linearity (R2≥0.999) in the corresponding concentration ranges. The limits of detection and quantitation of 30 PAHs were 0.10~1.83 μg/kg and 0.35~6.11 μg/kg respectively. The recoveries varied from 67.77% to 119.28% with relative standard deviation of 1.18~12.47% (n=6) at the spiked levels of 5, 20 and 50 μg/kg. The levels of 30 PAHs were investigated in 38 commercial edible vegetable oil samples which belong to 11 different species. The results showed that NAP, 2-MNAP, 1-MNAP, BIPH, DMNAP, ACY, ACE, TMNAP, FLU, DBTP, PHE, ANT, 1-MPHE, FLUR, PYR, CPP, BAA, CHR, BBF, BKF, BEP and BAP were detected in all samples; PER, 5-MCHR, ICDP, DBAHA, BGHIP and DBALP were detected with a ratio of 63.16%, 86.84%, 81.58%, 21.05%, 81.58% and 26.32% respectively; DBAEP and DBAHP were not detected in all samples. The total concentrations of 30 PAHs ranged from 92.56 μg/kg to 905.16 μg/kg, and concentrations of BAP varied from 1.94 μg/kg to 7.40 μg/kg which were at the safety levels according the limitation standard.

Key words: edible vegetable oil, removing fat through freezing, polycyclic aromatic hydrocarbons, gas chromatography - tandem mass spectrometry

中图分类号:

TS202.3

王国庆王宗义. 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, 0, (): 0-0.

Zong-Yi WANG. Determination of 30 Polycyclic Aromatic Hydrocarbons in Edible Vegetable Oils by Gas Chromatography – Tandem Mass Spectrometry with Removing fat through freezing[J]. FOOD SCIENCE, 0, (): 0-0.

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