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目的建立HPLC测定盐酸贝那替秦原料药及其注射剂的含量和有关物质的方法。方法以乙腈-磷酸二氢钾溶液(每1 000毫升含6.80 g磷酸二氢钾、0.556 g庚烷磺酸钠)35∶65为流动相;采用反相C18色谱柱,以1.0 mL/min流速,210 nm检测波长,30℃柱温,20μL进样量为色谱条件进行测定。结果盐酸贝那替秦原料药及注射液中各杂质峰峰面积之和不超过对照溶液主峰面积的1%;盐酸贝那替秦在浓度1~200μg/mL范围内具有良好线性关系(r=0.999 5),高、中、低浓度的平均回收率分别为98.99%(RSD=0.67%)、99.96%(RSD=0.10%)、101.21%(RSD=0.11%);日内(n=3)及日间精密度(n=5)RSD均小于2%,定量限1.7 ng,检测限0.4 ng。结论本实验方法专属性强、准确度高,可用于盐酸贝那替秦原料药和注射液的质量控制。
OBJECTIVE To establish a HPLC method for the determination of benazidine hydrochloride and its injections and its related substances. Methods The mobile phase consisted of acetonitrile - potassium dihydrogen phosphate solution (containing 6.80 g potassium dihydrogen phosphate and 0.556 g sodium heptane sulfonate per 1 000 ml) as mobile phase. The mobile phase was eluted with a reversed phase C18 column at a flow rate of 1.0 mL / min , 210 nm detection wavelength, 30 ℃ column temperature, 20μL injection volume for the chromatographic conditions were determined. Results The concentrations of the peak area of each impurity in the benazidine hydrochloride injection and the injection solution did not exceed 1% of the peak area of the control solution. Bentamine hydrochloride had a good linearity in the concentration range of 1 ~ 200 μg / mL (r = 0.999 5). The average recoveries of high, medium and low concentrations were 98.99% (RSD = 0.67%), 99.96% (RSD = 0.10%) and 101.21% (RSD = 0.11% The daytime precision (n = 5) RSD was less than 2%, the limit of quantification was 1.7 ng, and the limit of detection was 0.4 ng. Conclusion The experimental method is highly specific and accurate and can be used for the quality control of Benitalotide hydrochloride injection and injection.