Development and Validation of a Liquid Chromatography–Tandem Mass Spectrometry Method for Multiresidue Determination of 25 Herbicides in Soil and Tobacco

Abstract

In the cultivation of tobacco, crop rotation patterns, such as tobacco/rice or tobacco/corn, are widely used. However, the use of herbicides in the rice or corn phase can lead to their being taken in during the tobacco phase by inner conduction action. In the present study, to monitor the use of herbicides in tobacco, a sensitive and simple analytical method coupled with liquid chromatography-tandem mass spectrometry (LC–MS/MS) has been established for determination of 25 herbicides in soil as well as fresh and flue-cured tobacco leaf. The herbicides analyzed include six aryloxy phenoxy propionate herbicides (APPs) and 19 sulfonylureas herbicides (SUs). The samples were extracted using acetonitrile and purified using C18 sorbent before analysis. Optimum separation of the analytes was achieved using an Agilent Eclipse XDB-C18 column at 40 °C and gradient elution with acetonitrile and 0.1% aqueous formic acid as the mobile phase at a flow rate of 0.8 mL min−1. The limits of quantification and detection are in the ranges 0.08–1.00 mg kg−1 and 0.024–0.30 mg kg−1, respectively, and matrix effects in the range − 70 to 50% were achieved. The recovery rates obtained from spiked soil and tobacco leaf samples ranged from 72.32 to 116.83% with intra-day and inter-day relative standard deviations of 0.44–11.55%. In addition, the method developed was applied to the determination of herbicides residues in actual soil and tobacco samples, revealing that the proposed method can detect trace amounts of APPs and SUs in soil as well as in fresh and flue-cured tobacco leaf.