Optimization and Validation of a Multiresidue Method for Screening of 126 Pesticide Residues in Herbal Raw Materials and Extracts Used as Ingredients in Ayurvedic Medicines and Dietary Supplements

Abstract

Background Testing for pesticides levels in herbal products is an important aspect in determining product safety. Plants and its extracts are widely used as ingredients in botanical dietary supplements and traditional medicines. The extracts of plants, especially those prepared out of organic solvents are rich in secondary metabolites and pigments and adequate clean-up is required since the extracts completely dissolve in organic solvents. Objective The study aims at reporting a multi-residue analytical method for 126 different pesticides in raw material biomass as well as extracts of plants, which are widely used as ingredients in ayurvedic medicines as well as dietary supplements using LC-MSMS and GC-MSMS with a rugged sample preparation technique for accurate results. Method QuEChERS, GPC, GPC coupled with SPE and LLE coupled with SPE sample preparation methods were compared against each other for suitability to test pesticides in selected herbal raw materials and its alcoholic and aqueous extracts. The standard addition method was used for quantifying the level of pesticides below 10 μg/Kg. Results Single laboratory validation for sample preparation involving GPC and SPE resulted linearity in the range of 2.5–500 ng/mL, average intra-day and inter-day precision of 6.6% RSD, and average recovery (spiked at 10 μg/Kg) of 92% for all analytes tested. The method was repeatable with different analysts and days. Conclusions The sample preparation technique combining GPC and SPE as well as LLE and SPE were the most suitable for the selected herbal alcoholic extracts whereas any of the regular techniques involving LLE, SPE, and QuEChERS were suitable for raw material biomass as well as aqueous extracts. Highlights The method was found to be capable of determining selected pesticides in the selected matrices at 10 μg/Kg concentration. Provision of recycling solvents used in GPC+SPE method was adopted to make the method environmentally friendly.

Fast DLLME-GC-MS Method for Determination of Pesticides in Carmelite Drops and Evaluation of Matrix Effects in Related Medicinal Products

“…Furthermore, several investigations have revealed the exclusive existence of pesticides [ 13 , 14 , 15 ] in several dietary supplements, underscoring the need to assess the contamination profile of these commodities in light of their growing popularity and use. Uncontrolled pesticide use has negative effects and puts consumers at significant risk when it comes to commodities imported from underdeveloped countries [ 16 ].…”

“…Compared to other food products, there are fewer techniques available for the extraction and analysis of pesticides from plant-derived nutraceuticals [ 11 ]. Nutraceutical products have a very complex matrix in addition to being mostly concentrated plant forms, which means that large quantities of pigments, lipids, and other co-extractives are present [ 16 , 17 , 18 ]. A suitable sample preparation method and clean-up are necessary to separate and concentrate the target chemicals to detect pesticide residues.…”

High-throughput screening and quantification of pesticides in Lilii Bulbus using ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

“…The current screening technique commonly employed to address the intricate matrix of Chinese herbal materials and pesticides, with their unique properties, is low-resolution mass spectrometry. [18][19][20][21] However, this technique has limitations associated with retention time and scanning speed. To expand the scope of compounds detected, shorter retention times are necessary, but this compromises sensitivity and reproducibility.…”