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采用液相色谱-串联质谱法和气相色谱-串联质谱法综合测定葡萄叶片中的农药和植物生长调节剂残留量。

Comprehensive multiresidue determination of pesticides and plant growth regulators in grapevine leaves using liquid- and gas chromatography with tandem mass spectrometry.

机构信息

National Referral Laboratory, ICAR National Research Centre for Grapes, P.O. Manjri Farm, Pune, 412 307, India.

National Referral Laboratory, ICAR National Research Centre for Grapes, P.O. Manjri Farm, Pune, 412 307, India.

出版信息

J Chromatogr A. 2018 Dec 7;1579:73-82. doi: 10.1016/j.chroma.2018.10.025. Epub 2018 Oct 16.

Abstract

Grape leaf, which is known for its nutritional and medicinal properties, is finding increased applications for cuisine and remedial purposes. This article reports a comprehensive analytical method for the identification and quantification of a broad range of pesticides and plant growth regulators (PGRs) in the grape leaf matrix. The sample preparation method for pesticides involved an optimized QuEChERS-based extraction protocol, with subsequent clean-up by the dispersive solid phase extraction (dSPE) using a mixture of sorbents (25 mg PSA + 5 mg GCB + 150 mg MgSO). The PGRs were extracted with methanol. The performance of the method was investigated and validated for a mixture of 363 pesticides (148 in GC-MS/MS and 203 in LC-MS/MS) and 12 PGRs (LC-MS/MS) in compliance with the analytical quality control criteria of the SANTE/11813/2017 guidelines. The matrix effects were comparatively higher against grape berries. The findings indicated satisfactory recoveries at 10 ng/g and higher levels with precision RSDs less than 20%. This method has potential applications in commercial residue testing laboratories and also for the regulatory compliance check purposes for its lower LOQs compared to the corresponding EU-MRLs.

摘要

葡萄叶因其营养价值和药用特性而备受关注,在烹饪和医疗领域的应用也越来越广泛。本文报道了一种用于鉴定和定量分析葡萄叶基质中多种农药和植物生长调节剂(PGRs)的综合分析方法。该方法中,农药的样品前处理采用了基于 QuEChERS 的优化提取方案,随后使用混合吸附剂(25 mg PSA + 5 mg GCB + 150 mg MgSO)进行分散固相萃取(dSPE)净化。PGRs 则采用甲醇提取。该方法符合 SANTE/11813/2017 指南的分析质量控制标准,对 363 种农药(GC-MS/MS 法 148 种,LC-MS/MS 法 203 种)和 12 种 PGRs(LC-MS/MS 法)进行了性能考察和验证。与葡萄浆果相比,该方法对基质的干扰较大。结果表明,在 10 ng/g 及以上浓度下,回收率令人满意,精密度 RSD 小于 20%。与相应的欧盟最大残留限量(MRLs)相比,该方法的 LOQs 更低,因此具有在商业残留检测实验室中应用的潜力,也可用于法规遵从性检查。

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