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Simultaneous determination of corynoline and acetylcorynoline in human urine by LC-MS/MS and its application to a urinary excretion study.

Abstract

Corynoline and acetycorynoline, the major active components derived from Corydalis bungeana Herba, showed multiple pharmacological activities. However, quantification of the two compounds in human urine has not been reported. A simple liquid chromatography with tandem mass spectrometry method for the simultaneous determination of corynoline and acetycorynoline in human urine has been developed and fully validated. The analytes were extracted from urine samples by simple liquid-liquid extraction. Chromatographic separation was achieved on a Hedera ODS-2C18 column with the mobile phase of water (containing 0.5% formic acid) and acetonitrile (28:72, v/v) at a flow rate of 0.4mL/min. A tandem mass spectrometric detection was conducted using multiple reaction monitoring via an electrospray ionization source in positive mode. The monitored ion transitions were m/z 368.1→289.1 for corynoline, m/z 410.2→289.2 for acetycorynoline and m/z 380.2→243.2 for donepezil (internal standard), respectively. The calibration curves were linear (correlation coefficients>0.9970) over the concentration ranges of 3.0-3000pg/mL for corynoline and 3.0-1000pg/mL for acetycorynoline. The established method was highly sensitive with the lower limit of quantification (LLOQ) of 3.0pg/mL for both analytes. The intra- and inter-day precision was lower than 10% in terms of relative standard deviation for the low, medium, and high quality control samples, and lower than 16% for the LLOQ samples of the analytes. The accuracy was within ±10% in terms of relative error for both analytes. The method was successfully applied to a urinary excretion study after oral administration of the Chinese medicine formula Shuanghua Baihe tablets in healthy volunteers. The urinary excretion profiles of corynoline and acetycorynoline in human were first reported. The results of this study suggest that renal excretion was not the main excretion pathway of corynoline and acetycorynoline in humans.

Authors+Show Affiliations

Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China; Nanjing Clinical Tech Laboratories Inc., 18 Zhilan Road, Jiangning District, Nanjing 211000, China.National Key Institute of Traditional Chinese Medicine Quality Control, 1 South Yangtze River Road, Taizhou 25321, China.Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China; Nanjing Clinical Tech Laboratories Inc., 18 Zhilan Road, Jiangning District, Nanjing 211000, China.Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China; Nanjing Clinical Tech Laboratories Inc., 18 Zhilan Road, Jiangning District, Nanjing 211000, China.Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China; Nanjing Clinical Tech Laboratories Inc., 18 Zhilan Road, Jiangning District, Nanjing 211000, China.Yangtze River Pharmaceutical Group, Taizhou 25321, China.Institute of Dermatology, Chinese Academy of Medical Sciences & Peking Union Medical College, 12 Jiangwangmiao Street, Nanjing 210042, China. Electronic address: mpc815@163.com.Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China; Nanjing Clinical Tech Laboratories Inc., 18 Zhilan Road, Jiangning District, Nanjing 211000, China. Electronic address: dinglidl@hotmail.com.

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Study

Language

eng

PubMed ID

26882127

Citation

Liu, Ruijuan, et al. "Simultaneous Determination of Corynoline and Acetylcorynoline in Human Urine By LC-MS/MS and Its Application to a Urinary Excretion Study." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1014, 2016, pp. 83-9.
Liu R, Zheng L, Cheng M, et al. Simultaneous determination of corynoline and acetylcorynoline in human urine by LC-MS/MS and its application to a urinary excretion study. J Chromatogr B Analyt Technol Biomed Life Sci. 2016;1014:83-9.
Liu, R., Zheng, L., Cheng, M., Wu, Y., Gu, P., Liu, Y., Ma, P., & Ding, L. (2016). Simultaneous determination of corynoline and acetylcorynoline in human urine by LC-MS/MS and its application to a urinary excretion study. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1014, 83-9. https://doi.org/10.1016/j.jchromb.2016.01.046
Liu R, et al. Simultaneous Determination of Corynoline and Acetylcorynoline in Human Urine By LC-MS/MS and Its Application to a Urinary Excretion Study. J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Mar 1;1014:83-9. PubMed PMID: 26882127.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous determination of corynoline and acetylcorynoline in human urine by LC-MS/MS and its application to a urinary excretion study. AU - Liu,Ruijuan, AU - Zheng,Lu, AU - Cheng,Minlu, AU - Wu,Yao, AU - Gu,Pan, AU - Liu,Yujie, AU - Ma,Pengcheng, AU - Ding,Li, Y1 - 2016/02/02/ PY - 2015/09/16/received PY - 2015/11/22/revised PY - 2016/01/30/accepted PY - 2016/2/17/entrez PY - 2016/2/18/pubmed PY - 2016/11/10/medline KW - Acetycorynoline KW - Corynoline KW - Human urine KW - LC–MS/MS KW - Shuanghua Baihe tablets KW - Urinary excretion SP - 83 EP - 9 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 1014 N2 - Corynoline and acetycorynoline, the major active components derived from Corydalis bungeana Herba, showed multiple pharmacological activities. However, quantification of the two compounds in human urine has not been reported. A simple liquid chromatography with tandem mass spectrometry method for the simultaneous determination of corynoline and acetycorynoline in human urine has been developed and fully validated. The analytes were extracted from urine samples by simple liquid-liquid extraction. Chromatographic separation was achieved on a Hedera ODS-2C18 column with the mobile phase of water (containing 0.5% formic acid) and acetonitrile (28:72, v/v) at a flow rate of 0.4mL/min. A tandem mass spectrometric detection was conducted using multiple reaction monitoring via an electrospray ionization source in positive mode. The monitored ion transitions were m/z 368.1→289.1 for corynoline, m/z 410.2→289.2 for acetycorynoline and m/z 380.2→243.2 for donepezil (internal standard), respectively. The calibration curves were linear (correlation coefficients>0.9970) over the concentration ranges of 3.0-3000pg/mL for corynoline and 3.0-1000pg/mL for acetycorynoline. The established method was highly sensitive with the lower limit of quantification (LLOQ) of 3.0pg/mL for both analytes. The intra- and inter-day precision was lower than 10% in terms of relative standard deviation for the low, medium, and high quality control samples, and lower than 16% for the LLOQ samples of the analytes. The accuracy was within ±10% in terms of relative error for both analytes. The method was successfully applied to a urinary excretion study after oral administration of the Chinese medicine formula Shuanghua Baihe tablets in healthy volunteers. The urinary excretion profiles of corynoline and acetycorynoline in human were first reported. The results of this study suggest that renal excretion was not the main excretion pathway of corynoline and acetycorynoline in humans. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/26882127/Simultaneous_determination_of_corynoline_and_acetylcorynoline_in_human_urine_by_LC_MS/MS_and_its_application_to_a_urinary_excretion_study_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(16)30053-8 DB - PRIME DP - Unbound Medicine ER -