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| SPE-LC-MS/MS method for determination of hypoxanthine concentration in Shuxuetong injection |
| Hits 1511 Download times 1032 Received:May 20, 2019 |
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| DOI
10.11656/j.issn.1673-9043.2019.05.16 |
| Key Words
LC-MS/MS;solid phase extraction;Shuxuetong injection;hypoxanthine;quantitative determination |
| Author Name | Affiliation | E-mail | | WANG Xianrui | Tianjin University of Traditional Chinese Medicine, Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin 300193, China | | | ZHAO Xizi | Tianjin University of Traditional Chinese Medicine, Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin 300193, China | | | WANG Xiaoming | Tianjin University of Traditional Chinese Medicine, Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin 300193, China | | | GUO Yaqing | Tianjin University of Traditional Chinese Medicine, Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin 300193, China | | | PAN Guixiang | Second Affiliated Hospital of Tianjin University of Traditional Chinese Medicine, Tianjin 300250, China | guixiangp@163.com | | HUANG Yuhong | Second Affiliated Hospital of Tianjin University of Traditional Chinese Medicine, Tianjin 300250, China | |
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| Abstract
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| [Objective] Solid phase extraction with liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) was applied to determine the concentration of hypoxanthine in Shuxuetong injection.[Methods] After extracted with SPE column,Shuxuetong injection was detected by LC-MS/MS. This injection was separated on an Acquity BEH C18 column (100 mm×2.1 mm,1.7 μm),and methanol-water (containing 0.1% formic acid) was used as a mobile phase for gradient elution at a flow rate of 0.3 mL/min. Mass spectrometric detection was performed in negative ion and multiple reaction monitoring mode with an electrospray ionization (ESI) source. The ion pairs used for quantitative analysis were m/z 134.9→92.0 for hypoxanthine and m/z 151.0→92.1 for 6-mercaptopurine (internal standard,IS).[Results] Hypoxanthine had a good linear relationship with the peak area ratio of the analyte and the IS in the range of 0.1~0.5 μg/mL (r=0.999 8). The average recovery rate was 98.7%,and the RSD was 0.31%.[Conclusion] This method described here is a simple,accurate and sensitive method that can be used for the determination of hypoxanthine concentrationin Shuxuetong injection. |
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