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采用气相色谱-串联质谱法(GC-MS/MS)对种子香料孜然(Cuminum cyminum)和芫荽(Coriandrum sativum)中的农药残留进行多残留方法验证和安全性评估。

Multi-residue method validation and safety evaluation of pesticide residues in seed spices cumin (Cuminum cyminum) and coriander (Coriandrum sativum) by gas chromatography tandem mass spectrometry (GC-MS/MS).

机构信息

National Referral Laboratory, ICAR-National Research Centre for Grapes, Pune, Maharashtra 412307, India.

National Referral Laboratory, ICAR-National Research Centre for Grapes, Pune, Maharashtra 412307, India.

出版信息

Food Chem. 2022 Apr 16;374:131782. doi: 10.1016/j.foodchem.2021.131782. Epub 2021 Dec 7.

Abstract

The manuscript reports comprehensive multi-residue determination of 215 pesticides in two commercially important Indian spices, Cumin (Cuminum cyminum) and Coriander (Coriandrum sativum) by GC-MS/MS analysis. The proposed method involved liquid-liquid extraction with acetonitrile, d-SPE clean-up and final reconstitution of extract in ethyl acetate. d-SPE clean-up with PSA and C18 minimized the matrix effects by 40 and 16%, respectively. Reconstitution of final extract reduced the non-volatile matrix co-extractives by 36-40%. The method was validated as per SANTE/12682/2019 and recoveries at 10, 25 and 50 μg kg were within 70-120% with RSD ≤ 20%. A fit for purpose method LOQ of 10 μgkg was achieved for 85% of analytes. The method was successfully applied for comprehensive screening of cumin and coriander market samples. The calculated TMDI for acute and chronic exposure assessment were less than calculated MPI in respective matrices and therefore did not cause any adverse effect to consumers.

摘要

该手稿报告了通过 GC-MS/MS 分析对两种商业上重要的印度香料——孜然(Cuminum cyminum)和芫荽(Coriandrum sativum)中的 215 种农药进行的综合多残留测定。所提出的方法涉及用乙腈进行液液提取、d-SPE 净化和最终在乙酸乙酯中重新配制提取物。PSA 和 C18 的 d-SPE 净化分别将基质效应最小化了 40%和 16%。最终提取物的重新配制将非挥发性基质共提物减少了 36-40%。该方法按照 SANTE/12682/2019 进行了验证,在 10、25 和 50μgkg 的回收率在 70-120%之间,RSD≤20%。对于 85%的分析物,实现了针对性方法 LOQ 的 10μgkg。该方法成功应用于孜然和芫荽市场样品的综合筛选。在各自的基质中,计算出的急性和慢性暴露评估的 TMDI 均小于计算出的 MPI,因此不会对消费者造成任何不良影响。

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