HPLC法测定联苯苄唑原料药中的有关物质 点击下载
论文标题: HPLC法测定联苯苄唑原料药中的有关物质
英文标题:
中文摘要: 目的:建立测定联苯苄唑原料药中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Kromasil C18,流动相为甲醇-0.02 mol/L磷酸(用三乙胺调节pH至7.5)(70 ∶ 30,V/V),流速为1.0 ml/min,检测波长为258 nm,进样量为20 μl,柱温为40 ℃。结果:联苯苄唑、杂质A(联苯苄醇)和杂质B(4-C异构体)的检测质量浓度线性范围均为0.05~0.25 μg/ml(r分别为0.999 6、0.999 7、0.999 5);检测限分别为8.2、7.5、8.4 ng/ml,定量限分别为27.1、24.7、27.8 ng/ml;精密度、重复性试验的RSD<1%;杂质B加样回收率为95.13%~101.29%,RSD=1.89%(n=9);3批样品中均检出杂质A和杂质B。结论:该方法准确、灵敏度高、重复性好,可用于联苯苄唑原料药中有关物质的测定。
英文摘要: OBJECTIVE:To establish a method for the determination of related substances in bifonazole raw material. METHODS: HPLC method was performed on the column of Kromasil C18 with mobile phase of methanol-0.02 mol/L phosphoric acid (adjusted pH to 7.5 with triethylamine)(70 ∶ 30,V/V) at a flow rate of 1.0 ml/min, detection wavelength was 258 nm, volume injection was 20 μl,and the column temperature was 40 ℃. RESULTS:The linear range was 0.05-0.25 μg/ml for bifonazole(r=0.999 6),0.05-0.25 μg/ml for impurity A (bifonol)(r=0.999 7) and 0.05-0.25 μg/ml for impurity B (4-C isomer)(r=0.999 5); the detection limits were 8.2 ng/ml, 7.5 ng/ml and 8.4 ng/ml, and the quantification limits were 27.1 ng/ml, 24.7 ng/ml and 27.8 ng/ml, respectively; RSDs of precision and reproducibility tests were lower than 1%; recovery of impurity B was 95.13%-101.29%(RSD=1.89%,n=9); both impurity A and impurity B were were detected in the 3 batches of samples. CONCLUSIONS: The method is accurate, sensitive and reproducible, and can be used for the determination of the related substances in bifonazole raw material.
期刊: 2016年第27卷第12期
作者: 韩春晖,裘一兰,栾爽,耿欣
英文作者: HAN Chunhui,QIU Yilan,LUAN Shuang,GENG Xin
关键字: 高效液相色谱法;联苯苄唑原料药;有关物质
KEYWORDS: HPLC; Bifonazole raw material; Related substances
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