HPLC法测定硫酸卷曲霉素原料及其制剂中4个组分含量及有关物质
HPLC determination for the contents/components and related substances of capreomycin sulfate and its preparations
分类号：
出版年·卷·期（页码）：2014,34 (6):0-0
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要：-------------------------------------------------------------------------------------------
目的： 建立高效液相色谱法测定硫酸卷曲霉素原料及制剂中4个组分含量及有关物质。 方法： 采用Agela Venusuil XBP C18（L）（4.6 mm×250 mm，5 μm）色谱柱，流动相A为0.2 mol·L-1磷酸二氢钾+0.015 mol·L-1的己烷磺酸钠溶液（用磷酸溶液调节pH至2.3）-乙腈（93：7），流动相B为0.2 mol·L-1磷酸二氢钾+0.015 mol·L-1的己烷磺酸钠溶液（用磷酸溶液调节pH至2.3）-乙腈（90：10），梯度洗脱，流速1.0 mL·min-1，柱温25 ℃，检测波长为268 nm。 结果： 硫酸卷曲霉素含量测定，4个组分浓度在0.20~4.02 mg·mL-1内线性关系良好，制剂的平均回收率（n=9）为99.5%，定量限为0.03 μg；有关物质测定，硫酸卷曲霉素4个组分浓度在0.0086~0.0630 mg·mL-1内线性关系良好，检出限为0.01 μg；各杂质与硫酸卷曲霉素4个主成分色谱峰能完全分离。 结论： 经方法学验证，该方法可用于硫酸卷曲霉素原料及其制剂的质量控制。
-----英文摘要：---------------------------------------------------------------------------------------
Objective: To establish an HPLC method for the determination of the contents/components and related substances of capreomycin sulfate and its preparations. Methods: An Agela Venusuil XBP C18(L) column (4.6 mm×250 mm,5 μm) was used.The mobile phase A was 0.2 mol·L-1 potassium dihydrogen phosphate-0.015 mol·L-1 sodium hexanesulfonate,with phosphoric acid added to adjust the pH to 2.3-acetonitrile (93: 7);the mobile phase B was 0.2 mol·L-1 potassium dihydrogen phosphate-0.015 mol·L-1 sodium hexanesulfonate,with phosphoric acid added to adjust the pH to 2.3-acetonitrile (90: 10).The flow rate was 1.0 mL·min-1,the column temperature was 25 ℃ and the detection wavelength was 268 nm. Results: The linear rang of capreomycin for contents/components was 0.20-4.02 mg·mL-1.The average recovery(n=9) was 99.5% and the quantitative limit was 0.03 μg.The linear rang of capreomycin for related substances was 0.0086-0.0630 mg·mL-1 and the limit of detection was 0.01 μg.The related substances gained a completely chromatography separation with four principal peaks of capreomycin. Conclusion: Through the methodology validation,the method is accurate,sensitive and simple,which is a new reliable analytical method for the quality control of capreomycin sulfate and its preparations.
-----参考文献：---------------------------------------------------------------------------------------
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