伊曲康唑胶囊有关物质测定方法优化  

Optimization of Determination Method of the Related Substances in Itraconazole Capsules

作　　者：张秉华 杜亚俊 衷红梅 牛龙青 赵蒲中 ZHANG Binghua;DU Yajun;ZHONG Hongmei;NIU Longqing;ZHAO Puzhong(Shaanxi Institute for Food and Drug Control,Xi'an,Shaanxi,China 710065)

机构地区：[1]陕西省食品药品检验研究院,陕西西安710065

出　　处：《中国药业》2022年第14期75-78,共4页China Pharmaceuticals

基　　金：陕西省重点研发计划项目[2019SF-027];陕西省创新能力支撑计划项目[2020PT-041]。

摘　　要：目的优化伊曲康唑胶囊中有关物质的检测方法。方法色谱柱为Aglient Proshell 120 EC-C18柱(150 mm×4.6 mm,2.7μm),流动相为0.01 mol/L乙酸铵溶液-乙腈(梯度洗脱),流速为0.8 mL/min,检测波长为260 nm,柱温为30℃,进样量为10μL。对4家企业的12批样品进行检测,并将结果与2020年版《中国药典》有关物质检测方法结果进行比较。结果伊曲康唑、杂质B、杂质C、杂质D、杂质F、杂质G、杂质H质量浓度分别在0.3174~2.5396μg/mL,0.3118~2.4940μg/mL,0.2911~2.3286μg/mL,0.3067~2.4536μg/mL,0.3166~2.5324μg/mL,0.2860~2.2882μg/mL,0.3135~2.5078μg/mL范围内与峰面积线性关系良好(r>0.9995);检测限分别为0.38,0.37,0.35,0.37,0.38,0.57,1.25 ng,定量限分别为1.27,1.25,1.16,1.23,1.27,1.37,3.76 ng;重复性试验结果的RSD均小于3.85%(n=6);杂质B、杂质F、杂质G、杂质H的平均加样回收率分别为99.42%,99.54%,101.74%,105.96%,RSD分别为1.49%,1.79%,2.63%,6.98%(n=9)。4个企业共10批样品检测出上述杂质,且企业A检出杂质含量高于药典有关物质检测方法检出含量。结论该方法灵敏度高,分离效果及准确性好,可用于伊曲康唑胶囊有关物质的检测。Objective To optimize the determination method of related substances in Itraconazole Capsules.Methods The chromatographic column was Aglient Proshell 120 EC-C18 column(150 mm×4.6 mm,2.7μm),the mobile phase was 0.01 mol/L ammonium acetate solution-acetonitrile(gradient elution),the flow rate was 0.8 mL/min,the detection wavelength was 260 nm,the column temperature was 30℃,and the injection volume was 10μL.The content of related substances in 12 batches of samples from four manufacturers was determined,and the results were compared with the results determined by the test method for related substances in the Chinese Pharmacopoeia(2020 Edition).Results The linear ranges of itraconazole,impurity B,impurity C,impurity D,impurity F,impurity G and impurity H were 0.3174-2.5396μg/mL,0.3118-2.4940μg/mL,0.2911-2.3286μg/mL,0.3067-2.4536μg/mL,0.3166-2.5324μg/mL,0.2860-2.2882μg/mL and 0.3135-2.5078μg/mL(r>0.9995),respectively.The limits of detection(LOD)were 0.38,0.37,0.35,0.37,0.38,0.57 and 1.25 ng,respectively.The limits of quantitation(LOQ)were 1.27,1.25,1.16,1.23,1.27,1.37 and 3.76 ng,respectively.The RSD of the repeatability test was less than 3.85%(n=6).The average recoveries of impurity B,impurity F,impurity G and impurity H were 99.42%,99.54%,101.74%and 105.96%with RSDs of 1.49%,1.79%,2.63%and 6.98%(n=9),respectively.Impurities were detected in 10 batches of samples from four manufacturers,and the content of impurities in samples from manufacturer A detected by the established method was higher than that detected by the method for relevant substances in the Chinese Pharmacopoeia.Conclusion The method has high sensitivity,good separation effect and accuracy,which can be used for the determination of related substances in Itraconazole Capsules.

关 键 词：伊曲康唑胶囊 高效液相色谱法 有关物质 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]