Screening of pesticide residues in Traditional Chinese Medicines using modified QuEChERS sample preparation procedure and LC-MS/MS analysis

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Vol. 1152; p. 122224
• Main Authors: Li, Rui-Xing, Li, Min-Min, Wang, Tao, Wang, Tie-Lin, Chen, Jie-Yin, Francis, Frédéric, Fan, Bei, Kong, Zhi-Qiang, Dai, Xiao-Feng
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 01.09.2020
• Subjects: acetic acid; acetonitrile; China; Chromatography, High Pressure Liquid - methods; cortex; Drug Contamination; Drugs, Chinese Herbal - analysis; Drugs, Chinese Herbal - standards; habitats; Limit of Detection; Linear Models; liquid chromatography; magnesium sulfate; maximum residue limits; Medicine, Chinese Traditional; Modified QuEChERS; Multiresidues; Ophiopogon japonicus; Oriental traditional medicine; paclobutrazol; pesticide residues; Pesticide Residues - analysis; Pesticides; Reproducibility of Results; screening; sorbents; tandem mass spectrometry; Tandem Mass Spectrometry - methods; tebuconazole; Traditional Chinese Medicine; UHPLC-MS/MS; ultrasonic treatment; vegetables; China; Modified QuEChERS; UHPLC-MS/MS; Multiresidues; Pesticides; Traditional Chinese Medicine
• ISSN: 1570-0232; 1873-376X; 1873-376X
• DOI: 10.1016/j.jchromb.2020.122224

•108 pesticides in Traditional Chinese Medicines were determined simultaneously.•Traditional Chinese Medicines are difficult matrices for residue analysis.•C18 and anhydrous MgSO4 were used as the dSPE sorbent.•92% of real samples were detected with pesticide residues.•Paclobutrazol showed a high residue level in O. japonicas. A robust and high-throughput method was developed for the determination of 108 pesticide residues in Traditional Chinese Medicines (TCMs) simultaneously using a combination of UHPLC-MS/MS analysis and the modified QuEChERS method. Extraction was carried out in acetonitrile containing 0.75% (v/v) acetic acid with ultrasonication for 15 min; MgSO4 and C18 were used as the dispersive-solid phase extraction sorbents. The method exhibited good linearity (r2 > 0.9901), in addition to good selectivity, precision and repeatability. More than 92% of pesticides exhibited high rates or recovery in the 70–120% range. This method showed high sensitivity, with Limits of Quantitation in the 0.01–20 ng/mL range in Cortex Moutan, and 0.01–50 ng/mL in the other TCMs. The method was employed for the analysis of 39 real samples from different habitats, and pesticides were detected in 92.3% of the samples, with 26 pesticides being detected in these three TCMs. More than four pesticides were detected in a third of the samples. Among them, tebuconazole was detected in all the three TCMs with 0.22–22.02 μg/kg concentration, which was lower than the provisions in GB 2763-2019 (50 μg/kg). In addition, the paclobutrazol detection rate in Ophiopogon japonicus was 100%, and the detected concentrations of 9 samples exceeded the Maximum Residue Levels defined for vegetables (50 μg/kg). Considering there are no regulations that govern the limits of pesticide residues in the three TCMs in China, we recommend the acceleration of efforts to introduce appropriate regulations.