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Simultaneous determination of 35 ultra‐trace level organophosphorus pesticide residues in Sanjie Zhentong capsules of traditional Chinese medicine using ultra high performance liquid chromatography with tandem mass spectrometry
Author(s) -
Li Jiachun,
Li Dongpo,
Wu Jingling,
Qin Jianping,
Hu Junhua,
Huang Wenzhe,
Wang Zhenzhong,
Xiao Wei,
Wang Yu
Publication year - 2017
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201600570
Subject(s) - chromatography , chemistry , detection limit , sample preparation , analyte , gas chromatography/tandem mass spectrometry , solid phase extraction , tandem mass spectrometry , extraction (chemistry) , mass spectrometry , residue (chemistry) , biochemistry
The aim of this study was to develop an analytical method for the simultaneous determination of ultra‐trace levels of 35 organophosphorus pesticide residues in Sanjie Zhentong capsules, a traditional Chinese medicine prescription. A method based on multiclass and multiresidue sample preparation was developed. First, samples were hydrated with water at 4°C. A ratio of 1:3 sample/water was used for each of the sample amounts. Then, different extraction solvents were screened. This step was followed by a dispersive solid‐phase extraction clean‐up procedure using both primary secondary amine and polyamide. A comprehensive sensitive multiresidue liquid chromatography tandem mass spectrometry method was investigated and validated. Good linearity was achieved in the range of 10–500 μg/kg for each analyte. The average recovery ranged from 70 to 120%, except for methamidophos, fonophos, diazinon, and chlorpyriphos‐ethyl, the recoveries of which ranged from 60–70% at the lower concentration level. The precision values were lower than 10% for all the compounds in three concentration levels. The limits of detection and limits of quantification values were 0.01–2.1 and 0.05–3.4 μg/kg, respectively. The matrix effects were determined, and most of the compounds showed signal suppression. Finally, this optimized procedure was applied for the analysis of real samples.