Comparison of Electron Capture—Atmospheric Pressure Chemical Ionization and Electrospray Ionization for the Analysis of Gambogic Acid and its Main Circulating Metabolite in Dog Plasma

Author:

Yang Jing12,Ding Li12,Hu Linlin12,Jin Shaohong3,Liu Wenyuan12,Wang Zhenzhong4,Xiao Wei4,You Qidong5,Guo Qinglong5

Affiliation:

1. Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China

2. Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, 24 Tongjiaxiang, Nanjing 210009, China

3. National Institution for the Control of Pharmaceutical and Biological Products, Beijing 100050, China

4. Kanion Pharmaceutical Co. Ltd, Lianyungang 222001, China

5. Jiangsu Key Laboratory of Carcinogenesis and Intervention, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China

Abstract

Gambogic acid (GA), a promising anticancer candidate, is a polyprenylated xanthone abundant in the resin of Garcinia morella and Garcinia hanburyi. Electron capture–atmospheric pressure chemical ionization (EC-APCI) and electrospray ionization (ESI) techniques, both in the negative ion mode, were evaluated regarding ionization, fragmentation patterns and sensitivity for simultaneous liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis of GA and its main circulating metabolite, 10-hydroxygambogic acid (10-OHGA) in dog plasma. Both analytes underwent extensive in-source fragmentation in EC-APCI, which was not desirable for reliable quantification of these analytes, whereas the substitution of ESI for EC-APCI almost eliminated the source instability of both analytes. Negative ion ESI was, therefore, chosen for the development of an LC-MS/MS method for simultaneous determination of these analytes. After protein precipitation by acetonitrile, all analytes were separated on a Luna C18 HST column (50 × 2.0 mm i.d., 2.5 μm) with a mobile phase of 20 mmol L−1 ammonium acetate water solution containing 0.2% acetic acid: acetonitrile (18:82, v/v). The detection was performed on a tandem mass spectrometer using selective reaction monitoring mode. Calibration curves were linear over the range of 10–6000 ng mL−1 for GA and 3–2000 ng mL−1 for 10-OHGA. The method was successfully applied to the pharmacokinetics study of GA injection in six beagle dogs.

Publisher

SAGE Publications

Subject

Spectroscopy,Atomic and Molecular Physics, and Optics,General Medicine

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