Determination of nine organophosphorus pesticides by high-resolution hplc-ms/ms in medicinal plant materials

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Abstract

A method for the simultaneous determination of organophosphorus pesticides (OPPs)—diazinon, dimethoate, omethoate, pirimiphos-methyl, pirimiphos-ethyl, malathion, malaoxon, chlorpyrifos-methyl, and phosalone—in medicinal plant materials using high-resolution liquid chromatography-mass spectrometry has been developed. The method involves a rapid sample preparation procedure, where ground plant material is extracted with acetonitrile. Analytical conditions were optimized using reverse-phase chromatography. The determination is carried out using the internal standard method with deuterated standards of malathion-d6 and dichlorvos-d6, based on two of the most intense, specific ion reactions for each individual OPP. The method was tested on plant materials, specifically the rhizomes with roots of valerian (Rhizomata cum radicibus Valerianae officinalis), and validated for specificity, linearity, accuracy, analytical range, limit of quantification, precision, and matrix effect. This method can be used to determine the mentioned OPPs in a wide concentration range, from 0.01 to 10,000 ng/g of raw material, in both medicinal and agricultural plant cultivation.

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About the authors

O. V. Fateenkova

I.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation

Author for correspondence.
Email: Fateenkova-Olga@mail.ru
Russian Federation, Mosсow

A. M. Savvateev

I.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation

Email: Savvateev_A_M@staff.sechenov.ru
Russian Federation, Mosсow

A. V. Braun

Laboratory for the Chemical and Analytical Control of the Military Research Centre

Email: Fateenkova-Olga@mail.ru
Russian Federation, Moscow

V. L. Beloborodov

I.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation

Email: Fateenkova-Olga@mail.ru
Russian Federation, Moscow

I. V. Gravel

I.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation

Email: Fateenkova-Olga@mail.ru
Russian Federation, Mosсow

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2. Рис. 1. Масс-спектры фрагментаций протонированного молекулярного иона ометоата с m/z 214.0297, полученные в вариантах CID (25 B) и HCD (25 B). Режим регистрации положительных заряженных ионов.

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3. Рис. 2. Суперпозиция хроматограмм стандартного раствора, содержащего 100 нг/мл малатиона, по двум ионным реакциям. 1 – ионная реакция для определения содержания 214.0297 => 182.9875; 2 – ионная реакция для подтверждения присутствия 214.0297 => 196.0192.

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4. Схема 1. Структурные формулы фосфорорганических пестицидов.

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