顶空气相色谱法测定单磷酸阿糖腺苷中的残留溶剂

唐娜, 黄佳, 罗晶, 戴涌

中国医院药学杂志 ›› 2016, Vol. 36 ›› Issue (11) : 905-908.

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中国医院药学杂志 ›› 2016, Vol. 36 ›› Issue (11) : 905-908. DOI: 10.13286/j.cnki.chinhosppharmacyj.2016.11.08
研究论文

顶空气相色谱法测定单磷酸阿糖腺苷中的残留溶剂

  • 唐娜, 黄佳, 罗晶, 戴涌
作者信息 +

Determination of residual solvents in vidarabine monophosphate by headspace gas chromatography

  • TANG Na, HUANG Jia, LUO Jing, DAI Yong
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文章历史 +

摘要

目的: 建立测定单磷酸阿糖腺苷原料药中7种残留溶剂的顶空气相色谱法。方法: 使用DB-624毛细管柱(30m×0.32mm,1.8μm)为色谱柱,以水为溶剂,测定单磷酸阿糖腺苷原料中甲醇、乙醇、丙酮、乙腈、二氯甲烷、乙酸乙酯和吡啶的含量。结果: 甲醇、乙醇、丙酮、乙腈、二氯甲烷、乙酸乙酯和吡啶分离度好,在所考察的浓度范围内7种有机溶剂的峰面积与浓度呈良好的线性关系,相关系数在0.9979~0.9995之间;3个水平的回收率分别在81%~108%之间,各组分检出限在0.0497~0.499μg·mL-1之间。结论: 此方法准确、灵敏,可用于单磷酸阿糖腺苷原料药中残留溶剂的测定。

Abstract

OBJECTIVE To establish a method for determining seven residual solvents in vidarabine monophosphate by headspace gas chromatography.METHODS Residual solvents including methanol, ethanol, acetone, acetonitrile, dichloromethane, ethyl acetate and pyridine in vidarabine monophosphate were quantitatively determined on a DB-624 column (30 m×0.32 mm,1.8 μm), with water as solvent.RESULTS Seven residual solvents were completely separated. The method had a good linear relationship in proper concentration range and regression coefficients were between 0.997 9 and 0.999 5. Three levels of recovery were in range of 81%-108%. Detectable limit was 0.049 7-0.499 μg·mL-1.CONCLUSION This method is accurate and sensitive, which can be used for determination of residual solvents in vidarabine monophosphate.

关键词

单磷酸阿糖腺苷 / 残留溶剂 / 气相色谱法

Key words

vidarabine monphosphate / residual solvent / gas chromatography

引用本文

导出引用
唐娜, 黄佳, 罗晶, 戴涌. 顶空气相色谱法测定单磷酸阿糖腺苷中的残留溶剂[J]. 中国医院药学杂志, 2016, 36(11): 905-908 https://doi.org/10.13286/j.cnki.chinhosppharmacyj.2016.11.08
TANG Na, HUANG Jia, LUO Jing, DAI Yong. Determination of residual solvents in vidarabine monophosphate by headspace gas chromatography[J]. Chinese Journal of Hospital Pharmacy, 2016, 36(11): 905-908 https://doi.org/10.13286/j.cnki.chinhosppharmacyj.2016.11.08
中图分类号: R285   

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基金

陕西省科学技术发展计划(编号:2012K17-02-03)

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