| 引用本文: | 朱建喜,庄波阳,王凌,林敏.HPLC-MS/MS测定地高辛片中羟基洋地黄毒苷和洋地黄毒苷的含量[J].中国现代应用药学,2013,30(12):1342-1346. |
| ZHU Jianxi,ZHUANG Boyang,WANG Ling,LIN Min.Determination of Gitoxin and Digitoxin in Digaoxin Tablets by HPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2013,30(12):1342-1346. |
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| 摘要: |
| 目的 采用HPLC-MS/MS建立同时测定地高辛片中羟基洋地黄毒苷和洋地黄毒苷的方法。方法 色谱柱Agilent C18(150 mm×4.6 mm，5 μm)，流动相为乙腈-水(40∶60)，三重四极杆串联质谱检测，电喷雾离子化源(ESI)，在负离子条件下以多反应监测(MRM)方式进行扫描定量。结果 羟基洋地黄毒苷浓度在0.025 65~2.565 μg·mL-1内与峰面积呈良好的线性关系，r为0.999 3; 洋地黄毒苷浓度在0.025 95~2.596 μg·mL-1内与峰面积呈良好的线性关系，r为0.999 8；羟基洋地黄毒苷平均加样回收率为99.7%，RSD=2.2%；洋地黄毒苷平均加样回收率为100.9%，RSD=2.3%。结论 本方法简便、准确可靠，适用于地高辛片中羟基洋地黄毒苷和洋地黄毒苷两个主要有关物质的控制。 |
| 关键词: 地高辛片 液相色谱-串联质谱 有关物质 羟基洋地黄毒苷 洋地黄毒苷 |
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| Determination of Gitoxin and Digitoxin in Digaoxin Tablets by HPLC-MS/MS |
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ZHU Jianxi1, ZHUANG Boyang2, WANG Ling3, LIN Min2
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1.Nine-five Clinical Department Medical Device Division of Fuzhou General Hospital of Nanjing Military Command, Putian 351100, China;2.Fujian Provincial Institute for Drug Control, Fuzhou 350001, China;3.Department of Pharmacy, Provincial Clinical College of Fujian Medical University, Fujian Provincial Hospital, Fuzhou 350001, China
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| Abstract: |
| OBJECTIVE To establish an HPLC-MS/MS method for determining the contents of gitoxin and digitoxin in Digaoxin tablets. METHODS The condition of detection were: Agilent C18(150 mm×4.6mm, 5 μm), the mobile phase consisted of acetonitrile and water(40∶60), the detection wavelength was triple quadrupled tandem mass spectrometry with ESI source in the negative ion mode. Quantitation was performed using multiple reaction monitoring (MRM). RESULTS The calibration curves were linear in the range of 0.025 65-2.565 μg·mL-1 for gitoxin(r=0.999 3); the calibration curves were linear in the range of 0.025 95-2.596 μg·mL-1 for digitoxin(r=0.999 8). The average recovery of gitoxin was 99.7%(RSD=2.2%); the average recovery of digitoxin was 100.9%(RSD=2.3%). CONCLUSION The method is simple, accurate, reliable and can be used for the quality control of gitoxin and digitoxin in Digaoxin tablets. |
| Key words: Digaoxin tablets HPLC-MS/MS related substances gitoxin digitoxin |
