Abstract

Background

For years, turmeric has been used in several cuisines worldwide because of its proven health benefits. However, as its cultivation often involves applications of polar and semi-polar pesticides, their residues might cause health hazards to consumers. The dearth of a validated LC-MS/MS method for the residue analysis of these pesticides in turmeric has warranted the present study.

Objective

The aim was to develop and validate a multi-residue method for simultaneous determination of multi-class pesticides in turmeric (both rhizome and powder) by LC-MS/MS.

Method

Both the rhizome and powder samples (1 kg) were soaked in water for 30 min, followed by homogenization. Each homogenate (2 g) was mixed with 10 mL water, and extracted with acetonitrile (10 mL) in the presence of acetic acid and NaCl. The extract was cleaned by using dispersive solid phase extraction (dSPE) with graphitized carbon (5 mg/mL) sorbent. The cleaned extract was measured by LC-MS/MS with a runtime of 20 min. The method was validated on 211 multi-class pesticides.

Results

The method performance was satisfactory at 10 ng/g and higher levels, in compliance with the SANTE/12682/2019 guidelines. The dSPE cleanup was effective in minimizing the matrix effects. The use of matrix-matched calibrations specific for turmeric powder and rhizome corrected all recoveries within the satisfactory range of 70–120%. The precision -RSDs were <20% for all test pesticides. The Horwitz ratio and measurement uncertainty results were satisfactory as well.

Conclusions

As the method was convenient, selective, accurate, and repeatable, it is recommended for regulatory and commercial testing purposes.

Highlights

For the first time, this study reports a validated LC-MS/MS method for the multi-residue analysis of pesticides in turmeric. The method provided a high throughput analysis of multi-class pesticides in turmeric rhizome and powder matrices with satisfactory selectivity, sensitivity, accuracy, and precision. The method performance satisfied the requirements of the SANTE/12682/2019 guidelines, and the method sensitivity complied with the EU-MRL requirements.

中文翻译：

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液相色谱串联质谱法同时分析姜黄中多种农药的多残留方法的单实验室验证

抽象的

背景

多年来，姜黄因其对健康的益处而被广泛用于世界各地的多种美食中。但是，由于其种植经常涉及极性和半极性农药的使用，因此其残留物可能对消费者造成健康危害。缺乏用于姜黄中这些农药残留分析的有效LC-MS / MS方法值得进行本研究。

客观的

目的是开发和验证一种通过LC-MS / MS同时测定姜黄中的多种农药（根茎和粉末）的多残留方法。

方法

将根茎和粉末样品（1千克）均浸入水中30分钟，然后均质化。将每种匀浆（2 g）与10 mL水混合，并在乙酸和NaCl存在下，用乙腈（10 mL）萃取。通过使用分散固相萃取（dSPE）和石墨化碳（5 mg / mL）吸附剂清洁萃取液。清洁的萃取物通过LC-MS / MS测量，运行时间为20分钟。该方法在211种多类农药上得到了验证。

结果

符合SANTE / 12682/2019指南，该方法的性能在10 ng / g和更高水平上令人满意。dSPE净化可有效降低基质效应。使用姜黄粉和根茎特有的基质匹配校准物校正了所有回收率，均在70-120％的令人满意的范围内。所有测试农药的精密度-RSDs <20％。Horwitz比率和测量不确定度结果也令人满意。

结论

由于该方法方便，选择性，准确和可重复，因此建议用于监管和商业测试目的。

强调

这项研究首次报告了一种经过验证的LC-MS / MS方法，用于姜黄中农药的多残留分析。该方法对姜黄根茎和粉末基质中的多种农药进行了高通量分析，具有良好的选择性，灵敏度，准确性和精密度。方法性能满足SANTE / 12682/2019准则的要求，并且方法灵敏度符合EU-MRL要求。