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Simultaneous determination of three pesticide adjuvant residues in plant-derived agro-products using liquid chromatography-tandem mass spectrometry.

Journal of chromatography. A (2017-11-07)
Hui Li, Zejun Jiang, Xiaolin Cao, Hang Su, Hua Shao, Fen Jin, A M Abd El-Aty, Jing Wang
ABSTRACT

Herein, an accurate and reliable isotope-labelled internal standard method was developed and validated for simultaneous determination of three polar pesticide adjuvants, namely 2-pyrrolidone, N-methyl-2-pyrrolidone, and N-ethyl-2-pyrrolidone in plant-derived agro-products. Matrices, including apple, cabbage, tomato, cucumber, rice, and wheat were extracted with a modified quick, easy, cheap, effective, rugged, and safe "QuEChERS" method and purified with a new clean-up sorbent (Z-Sep). A hydrophilic interaction liquid chromatography column (HILIC), exhibiting a lipophilic-hydrophilic character, was used to separate the three analytes over 10min using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Matrix effects in various matrices were evaluated and an isotope-labelled internal standard method was employed to compensate for ion enhancement/suppression effects. At three fortification levels (2.0, 5.0, and 20.0μg/kg), the mean recoveries ranged from 78.5 to 112.1% with relative standard deviations (RSDs)<11.0% for all tested analytes. The limits of detection (LODs) and quantification (LOQs) were 0.04-0.45 and 0.12-1.58μg/kg in various matrices, respectively. The developed experimental protocol was successfully applied to monitor different samples purchased from local markets in Beijing, China. In conclusion, the developed method exhibited both high sensitivity and satisfactory accuracy and is suitable for the simultaneous determination of the three tested pesticide adjuvant residues in agro-products of plant origin.

MATERIALS
Product Number
Brand
Product Description

Supelco
Supel QuE, Z-Sep+ Bulk, pkg of 20 g
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep/C18 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Bulk
Supelco
Supel QuE, Z-Sep/C18 Tube, centrifuge tube volume 2 mL, pack of 100
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep+ Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep Tube, centrifuge tube volume 2 mL, pack of 100 ea
Sigma-Aldrich
L-Pyroglutamic acid 2-naphthylamide, ≥99% (TLC)
Sigma-Aldrich
1-Ethyl-2-pyrrolidone, 98%