Screening of pesticide residues in Traditional Chinese Medicines using modified QuEChERS sample preparation procedure and LC-MS/MS analysis
•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 re...
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| Published in | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Vol. 1152; p. 122224 |
|---|---|
| Main Authors | , , , , , , , , |
| Format | Journal Article |
| Language | English |
| Published |
Netherlands
Elsevier B.V
01.09.2020
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| Subjects | |
| Online Access | Get full text |
| ISSN | 1570-0232 1873-376X 1873-376X |
| DOI | 10.1016/j.jchromb.2020.122224 |
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| Abstract | •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. |
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| AbstractList | •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. 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.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. 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. 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; MgSO and C18 were used as the dispersive-solid phase extraction sorbents. The method exhibited good linearity (r > 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. |
| ArticleNumber | 122224 |
| Author | Fan, Bei Kong, Zhi-Qiang Li, Rui-Xing Wang, Tie-Lin Chen, Jie-Yin Francis, Frédéric Dai, Xiao-Feng Li, Min-Min Wang, Tao |
| Author_xml | – sequence: 1 givenname: Rui-Xing surname: Li fullname: Li, Rui-Xing organization: Key Laboratory of Agro-products Quality and Safety Control in Storage and Transport Process, Ministry of Agriculture and Rural Affairs/Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China – sequence: 2 givenname: Min-Min surname: Li fullname: Li, Min-Min organization: Key Laboratory of Agro-products Quality and Safety Control in Storage and Transport Process, Ministry of Agriculture and Rural Affairs/Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China – sequence: 3 givenname: Tao surname: Wang fullname: Wang, Tao organization: Institute of Chinese Medicinal Materials, Mianyang Academy of Agricultural Sciences, Mianyang 621023, PR China – sequence: 4 givenname: Tie-Lin surname: Wang fullname: Wang, Tie-Lin organization: National Resource Center for Chinese Materia Medica, China Academy of Chinese Medical Sciences, State Key Laboratory Breeding Base of Dao-di Herbs, Beijng 100700, PR China – sequence: 5 givenname: Jie-Yin surname: Chen fullname: Chen, Jie-Yin organization: Key Laboratory of Agro-products Quality and Safety Control in Storage and Transport Process, Ministry of Agriculture and Rural Affairs/Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China – sequence: 6 givenname: Frédéric surname: Francis fullname: Francis, Frédéric organization: Gembloux Agro-Bio-Tech, University of Liège, Passage des Déportés 2, 5030 Gembloux, Belgium – sequence: 7 givenname: Bei surname: Fan fullname: Fan, Bei email: fanbeicaas@163.com organization: Key Laboratory of Agro-products Quality and Safety Control in Storage and Transport Process, Ministry of Agriculture and Rural Affairs/Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China – sequence: 8 givenname: Zhi-Qiang surname: Kong fullname: Kong, Zhi-Qiang email: kongzhiqiang@caas.cn organization: Key Laboratory of Agro-products Quality and Safety Control in Storage and Transport Process, Ministry of Agriculture and Rural Affairs/Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China – sequence: 9 givenname: Xiao-Feng surname: Dai fullname: Dai, Xiao-Feng email: daixiaofeng_caas@126.com organization: Key Laboratory of Agro-products Quality and Safety Control in Storage and Transport Process, Ministry of Agriculture and Rural Affairs/Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China |
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| Keywords | Modified QuEChERS UHPLC-MS/MS Multiresidues Pesticides Traditional Chinese Medicine |
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| Snippet | •108 pesticides in Traditional Chinese Medicines were determined simultaneously.•Traditional Chinese Medicines are difficult matrices for residue analysis.•C18... A robust and high-throughput method was developed for the determination of 108 pesticide residues in Traditional Chinese Medicines (TCMs) simultaneously using... |
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| SubjectTerms | 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 |
| Title | Screening of pesticide residues in Traditional Chinese Medicines using modified QuEChERS sample preparation procedure and LC-MS/MS analysis |
| URI | https://dx.doi.org/10.1016/j.jchromb.2020.122224 https://www.ncbi.nlm.nih.gov/pubmed/32559653 https://www.proquest.com/docview/2415302303 https://www.proquest.com/docview/2985989930 |
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