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An effective methodology for simultaneous quantification of thiophanate-methyl, and its metabolite carbendazim in pear, using LC-MS/MS.

Abstract

Herein we have developed an optimized analytical method for the simultaneous quantification of a fungicide, thiophanate-methyl, and its metabolite, carbendazim, in pear cultivated under open-field conditions using liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). Due to the problem of partitioning associated with using acetonitrile and salts, methanol was used for sample extraction; the extract was then filtered using a vacuum filter, and cleaned-up using C18 QuEChERS bulk sorbent following dispersive solid-phase extraction (d-SPE) procedure. Since a common problem, "matrix effect", associated with the matrix was observed in LC-MS/MS, calibration curves for both thiophanate-methyl and carbendazim were constructed in the matrix using seven different concentration levels. Excellent linearity was observed, with determinant coefficient (R2) ≥ 0.9990. The limits of quantification (LOQs) were ≤0.02 mg/kg, satisfactory in terms of the maximum residue limits. Methods were validated at two fortification concentrations (10 × LOQ and 50 × LOQ); the experiments were repeated three times for each level and the average recoveries were 75.00-84.92%, with the coefficient of variation (CV) being ≤5.78%. The developed analytical method was applied to pear samples previously sprayed with commercial thiophanate-methyl formulation four times on different days during pre-harvest treatment. The parent compound was converted to its metabolites and the total residues degraded continuously until harvest. The data obtained in this study could help set safety guidelines for thiophanate-methyl in pear.

Authors+Show Affiliations

Natural Products Chemistry Laboratory, Chonnam National University, Yongbong-ro 77, Buk-gu, Gwangju 500-757, Republic of Korea.Natural Products Chemistry Laboratory, Chonnam National University, Yongbong-ro 77, Buk-gu, Gwangju 500-757, Republic of Korea. Electronic address: musfiq_707@yahoo.com.Natural Products Chemistry Laboratory, Chonnam National University, Yongbong-ro 77, Buk-gu, Gwangju 500-757, Republic of Korea.Natural Products Chemistry Laboratory, Chonnam National University, Yongbong-ro 77, Buk-gu, Gwangju 500-757, Republic of Korea.Rural and Bio-System Engineering, College of Agriculture and Life Science, Chonnam National University, Yongbong-ro 77, Buk-gu, Gwangju 500-757, Republic of Korea.National Agricultural Products Quality Management Service, Ministry of Agriculture, Food and Rural Affairs, 141, Yongjeon-ro, Gimcheon-Si, Gyeongsangbuk-do 39660, Republic of Korea.Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211 Giza, Egypt.Natural Products Chemistry Laboratory, Chonnam National University, Yongbong-ro 77, Buk-gu, Gwangju 500-757, Republic of Korea. Electronic address: jhshim@jnu.ac.kr.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

30031944

Citation

Lee, Han Sol, et al. "An Effective Methodology for Simultaneous Quantification of Thiophanate-methyl, and Its Metabolite Carbendazim in Pear, Using LC-MS/MS." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1095, 2018, pp. 1-7.
Lee HS, Rahman MM, Chung HS, et al. An effective methodology for simultaneous quantification of thiophanate-methyl, and its metabolite carbendazim in pear, using LC-MS/MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2018;1095:1-7.
Lee, H. S., Rahman, M. M., Chung, H. S., Kabir, H., Yoon, K. S., Cho, S. K., Abd El-Aty, A. M., & Shim, J. H. (2018). An effective methodology for simultaneous quantification of thiophanate-methyl, and its metabolite carbendazim in pear, using LC-MS/MS. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1095, 1-7. https://doi.org/10.1016/j.jchromb.2018.07.010
Lee HS, et al. An Effective Methodology for Simultaneous Quantification of Thiophanate-methyl, and Its Metabolite Carbendazim in Pear, Using LC-MS/MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Sep 15;1095:1-7. PubMed PMID: 30031944.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - An effective methodology for simultaneous quantification of thiophanate-methyl, and its metabolite carbendazim in pear, using LC-MS/MS. AU - Lee,Han Sol, AU - Rahman,Md Musfiqur, AU - Chung,Hyung Suk, AU - Kabir,Humayun, AU - Yoon,Kwang-Sik, AU - Cho,Soon-Kil, AU - Abd El-Aty,A M, AU - Shim,Jae-Han, Y1 - 2018/07/19/ PY - 2018/05/27/received PY - 2018/07/09/revised PY - 2018/07/10/accepted PY - 2018/7/23/pubmed PY - 2018/10/10/medline PY - 2018/7/23/entrez KW - Carbendazim KW - LC-MS/MS KW - Metabolite KW - Pear KW - Thiophanate-methyl SP - 1 EP - 7 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 1095 N2 - Herein we have developed an optimized analytical method for the simultaneous quantification of a fungicide, thiophanate-methyl, and its metabolite, carbendazim, in pear cultivated under open-field conditions using liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). Due to the problem of partitioning associated with using acetonitrile and salts, methanol was used for sample extraction; the extract was then filtered using a vacuum filter, and cleaned-up using C18 QuEChERS bulk sorbent following dispersive solid-phase extraction (d-SPE) procedure. Since a common problem, "matrix effect", associated with the matrix was observed in LC-MS/MS, calibration curves for both thiophanate-methyl and carbendazim were constructed in the matrix using seven different concentration levels. Excellent linearity was observed, with determinant coefficient (R2) ≥ 0.9990. The limits of quantification (LOQs) were ≤0.02 mg/kg, satisfactory in terms of the maximum residue limits. Methods were validated at two fortification concentrations (10 × LOQ and 50 × LOQ); the experiments were repeated three times for each level and the average recoveries were 75.00-84.92%, with the coefficient of variation (CV) being ≤5.78%. The developed analytical method was applied to pear samples previously sprayed with commercial thiophanate-methyl formulation four times on different days during pre-harvest treatment. The parent compound was converted to its metabolites and the total residues degraded continuously until harvest. The data obtained in this study could help set safety guidelines for thiophanate-methyl in pear. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/30031944/An_effective_methodology_for_simultaneous_quantification_of_thiophanate_methyl_and_its_metabolite_carbendazim_in_pear_using_LC_MS/MS_ DB - PRIME DP - Unbound Medicine ER -