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采用双气相色谱系统(GC-脉冲火焰光度法和保留时间锁定 GC-质谱法)对黄瓜中有机磷农药残留进行定性分析的新方法。

A new approach to qualitative analysis of organophosphorus pesticide residues in cucumber using a double gas chromatographic system: GC-pulsed-flame photometry and retention time locking GC-mass spectrometry.

机构信息

Laboratory of Chemical Analysis, Alhóndiga La Unión SAT, E-4700 El Ejido, Almeria, Spain.

出版信息

Talanta. 2003 Jun 13;60(2-3):433-47. doi: 10.1016/S0039-9140(03)00108-5.

Abstract

A qualitative method for the screening of organophosphorus pesticides (OPs) that could present in different types of vegetables has been established and validated. A typical multi-residue extraction procedure of OPs using ethyl acetate and sodium sulphate has been applied. No clean-up was required after extraction, and concentrated extracts were analysed by gas chromatography with pulsed-flame photometric detection (GC-PFPD). Confirmation of compound identities was performed by gas chromatography with mass spectrometric detection (GC-MSD) in the electron impact (EI) mode with full scan acquisition. Retention time locking (RTL) software was used in order to improve the method capability of identification and confirmation. Spiked samples at pesticide concentrations equal to the maximum residue level (MRL) were used to check chromatographic performance and for validation studies. The proposed method allows a rapid and accurate identification of the studied OPs until the ng ml(-1) range for those whose use is forbidden, and above their MRL concentration for the rest.

摘要

建立并验证了一种可用于筛选不同类型蔬菜中存在的有机磷农药(OPs)的定性方法。采用乙酸乙酯和硫酸钠的典型多残留 OP 提取程序。提取后无需净化,浓缩提取物用气相色谱法与脉冲火焰光度检测(GC-PFPD)进行分析。通过电子轰击(EI)模式全扫描采集的气相色谱-质谱检测(GC-MSD)对化合物的身份进行确认。使用保留时间锁定(RTL)软件可提高该方法的识别和确认能力。使用浓度等于最大残留限量(MRL)的农药添加样品来检查色谱性能并进行验证研究。该方法可快速准确地识别研究中的 OPs,直至禁用的 OPs 达到 ng ml(-1) 范围,其余 OPs 则达到其 MRL 浓度以上。

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