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采用气相色谱-串联质谱法对姜黄(粉末和根茎)中的农药多残留进行分析。

Multi-residue Analysis of Pesticides in Turmeric (Powder and Rhizome) Using Gas Chromatography Tandem Mass Spectrometry.

机构信息

National Referral Laboratory, ICAR-National Research Centre for Grapes, P.O. Manjri Farm, Pune 412307, India.

Agilent Technologies, Bangalore 560048, India.

出版信息

J AOAC Int. 2020 Nov 1;103(6):1498-1511. doi: 10.1093/jaoacint/qsaa078.

Abstract

BACKGROUND AND OBJECTIVES

Turmeric is widely used as an ingredient of food and medicinal products. There exists no validated method for multi-residue analysis of pesticides in turmeric.

OBJECTIVE

This study was undertaken to develop a simple and robust method for the quantitative determination of multi-class pesticides in turmeric powder and rhizome by GC-MS/MS.

METHOD

Initially, the samples were soaked in water for 30 min and homogenized to a fine paste. A portion of this paste (2 g) was extracted with acetonitrile (2 mL) and partitioned with hexane (2 mL) after adding 5 mL of 20% NaCl. The cleanup step involved dispersive solid phase extraction with graphitized carbon black (GCB, 5 mg/mL). Its performance was evaluated against primary secondary amine (PSA) and C18 sorbents. The cleaned extract was evaporated to dryness and reconstituted in ethyl acetate before GC-MS/MS analysis. The method was validated for a mixture of 208 multi-class pesticides at 10 ng/g and higher levels (i.e., 20 and 50 ng/g).

RESULTS

The findings, which demonstrated a satisfactory recovery and precision (RSDs <20%) for all compounds at 10 ng/g and higher spiking levels, are aligned with the analytical quality control criteria of SANTE/12682/2019 guidelines. The cleanup effect of GCB was much superior to that of PSA, C18, and their combinations. The solvent exchange step with hexane was effective in removing co-extractives and minimizing matrix effects.

CONCLUSIONS

This method complies with the regulatory requirements and is fit-for-purpose for pesticide residue monitoring in turmeric.

HIGHLIGHTS

The study reports a validated GC-MS/MS method for multi-residue analysis of pesticides in turmeric for the first time. The method provided a high throughput analysis of multi-class pesticides in turmeric rhizome and powder matrices with satisfactory selectivity, sensitivity, accuracy, and precision.

摘要

背景与目的

姜黄作为食品和药用产品的一种成分被广泛使用。目前还没有经过验证的方法可以用于分析姜黄中的多残留农药。

目的

本研究旨在建立一种简单、稳健的方法,用于通过气相色谱-串联质谱法(GC-MS/MS)定量测定姜黄粉和根茎中的多类农药残留。

方法

首先,将样品浸泡在水中 30 分钟,然后将其均质成细浆。取一部分该浆(2 克),用乙腈(2 毫升)提取,加入 5 毫升 20%氯化钠后,用正己烷(2 毫升)萃取。净化步骤包括使用石墨化炭黑(GCB,5 毫克/毫升)进行分散固相萃取。将其与初级二级胺(PSA)和 C18 吸附剂进行性能比较。将净化后的提取物蒸发至干,用乙酸乙酯重新溶解,然后进行 GC-MS/MS 分析。该方法在 10ng/g 及以上浓度(即 20ng/g 和 50ng/g)下对 208 种多类农药混合物进行了验证。

结果

在 10ng/g 及以上加标水平下,所有化合物的回收率和精密度(RSDs<20%)均令人满意,结果符合 SANTE/12682/2019 指南分析质量控制标准。GCB 的净化效果明显优于 PSA、C18 及其组合。用正己烷进行溶剂交换步骤可以有效地去除共提取物并最大限度地减少基质效应。

结论

该方法符合法规要求,适用于姜黄中农药残留的监测。

重点

本研究首次报道了一种用于姜黄中多残留农药分析的经验证的 GC-MS/MS 方法。该方法对姜黄根茎和粉末基质中的多类农药进行了高通量分析,具有较高的选择性、灵敏度、准确性和精密度。

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