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串联质谱在食品安全评估中的应用:橄榄油中邻苯二甲酸酯的测定

Tandem mass spectrometry in food safety assessment: the determination of phthalates in olive oil.

作者信息

Cavaliere Brunella, Macchione Barbara, Sindona Giovanni, Tagarelli Antonio

机构信息

Dipartimento di Chimica, Università della Calabria, Via P. Bucci, Cubo 12/C, I-87030 Arcavacata di Rende (CS), Italy.

出版信息

J Chromatogr A. 2008 Sep 26;1205(1-2):137-43. doi: 10.1016/j.chroma.2008.08.009. Epub 2008 Aug 7.

Abstract

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method for the detection of six phthalates in olive oil was developed. A gel permeation chromatography (GPC) clean-up step with cyclohexane:dichoromethane 7:3 as mobile phase was employed to remove the high-molecular mass species present in oil. Two ionization methodologies, i.e. electron (EI) and isobutane-chemical ionization (CI), were compared, in MS/MS mode, to achieve better analytical performances. An overall evaluation of all analytical parameters shows that the EI-MS/MS approach provides satisfactory results and is to be preferred to CI-MS/MS, at least in the case of the examined analytes. The observed accuracies, ranging from 71.7% to 112.2%, and the RSD values less than 9.7%, confirm the effectiveness of the proposed method in the assay of phthalate content in such a complex matrix as olive oil. The proposed protocol for the identification and assay of phthalates in olive oil might be of interest for the implementation of the QS (quality assurance scheme) for residue monitoring in food safety assessment.

摘要

建立了一种气相色谱 - 串联质谱(GC-MS/MS)法检测橄榄油中的六种邻苯二甲酸酯。采用以环己烷:二氯甲烷7:3为流动相的凝胶渗透色谱(GPC)净化步骤,去除油中存在的高分子量物质。在MS/MS模式下,比较了两种电离方法,即电子电离(EI)和异丁烷化学电离(CI),以获得更好的分析性能。对所有分析参数的综合评估表明,EI-MS/MS方法能提供令人满意的结果,至少在所检测的分析物情况下,比CI-MS/MS更可取。观察到的准确度在71.7%至112.2%之间,相对标准偏差(RSD)值小于9.7%,证实了该方法在检测橄榄油这种复杂基质中邻苯二甲酸酯含量方面的有效性。所提出的橄榄油中邻苯二甲酸酯鉴定和测定方案可能对食品安全评估中实施残留物监测的质量保证计划(QS)具有重要意义。

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