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气相色谱/单四极杆和串联质谱稳定同位素稀释法测定环氧大豆油

Determination of epoxidized soybean oil by gas chromatography/single quadrupole and tandem mass spectrometry stable isotope dilution assay.

作者信息

Rothenbacher Thorsten, Schwack Wolfgang

机构信息

Chemisches und Veterinäruntersuchungsamt Stuttgart, Schaflandstrasse 3/2, 70736 Fellbach, Germany.

出版信息

Rapid Commun Mass Spectrom. 2007;21(12):1937-43. doi: 10.1002/rcm.3033.

Abstract

PVC lids of glass jars often contain epoxidized soybean oil (ESBO), able to migrate and contaminate food. To establish a stable isotope dilution assay (SIDA), the 13C18-labelled internal standard ethyl 9,10,12,13-diepoxyoctadecanoate (13C(18:2E)Et) was synthesized, providing after sample preparation the same retention time as methyl 9,10,12,13-diepoxyoctadecanoate ((18:2E)Me), commonly used as a marker for ESBO in gas chromatographic (GC) analysis. For eleven different food matrices, the GC capillary columns VF-17ms, DB1701 and DB1 were tested with single quadrupole (GC/MS) as well as tandem mass spectrometric detection (GC/MS/MS). Overall, the VF-17ms column coupled with MS/MS detection showed the best results in terms of separation and sensitivity. The method validation for the matrix spiked olive oil resulted in a limit of detection (LOD) of 5 mg kg-1, a limit of quantification (LOQ) of 11 mg kg-1, a mean recovery (n=5, c=106.5 mg kg-1) of 99.7+/-5.5%, with a repeatability (within-run precision) of 6.0%. By means of GC/MS an LOQ of 21 mg kg-1 and a mean recovery (n=5, c=106.5 mg kg-1) of 103.3+/-0.8% with a repeatability of 0.9% were determined.

摘要

玻璃罐的聚氯乙烯盖子通常含有环氧大豆油(ESBO),这种物质能够迁移并污染食品。为建立一种稳定同位素稀释分析方法(SIDA),合成了13C18标记的内标物9,10,12,13-二环氧十八烷酸乙酯(13C(18:2E)Et),在样品制备后,其保留时间与气相色谱(GC)分析中常用作ESBO标记物的9,10,12,13-二环氧十八烷酸甲酯((18:2E)Me)相同。对于11种不同的食品基质,使用单四极杆(GC/MS)以及串联质谱检测(GC/MS/MS)对VF-17ms、DB-1701和DB-1气相色谱毛细管柱进行了测试。总体而言,结合MS/MS检测的VF-17ms柱在分离和灵敏度方面表现出最佳结果。对添加了基质的橄榄油进行方法验证,得到的检测限(LOD)为5 mg kg-1,定量限(LOQ)为11 mg kg-1,平均回收率(n = 5,c = 106.5 mg kg-1)为99.7±5.5%,重复性(批内精密度)为6.0%。通过GC/MS测定,定量限为21 mg kg-1,平均回收率(n = 5,c = 106.5 mg kg-1)为103.3±0.8%,重复性为0.9%。

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