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目的:研究建立高效液相色谱法(high performance liquid chromatography,HPLC)测定地拉罗司有关物质的方法。方法:采用CAPCELL PAK C18MGⅡ色谱柱(250 mm×4.6 mm,5μm),以0.05 mol·L-1磷酸二氢钠溶液(磷酸调至p H 3.5)为流动相A、乙腈为流动相B进行梯度洗脱,检测波长为245 nm,流速为1.0 m L·min-1。结果:地拉罗司与原料、中间体及其他杂质峰分离良好;地拉罗司的线性范围为0.1~40μg·m L-1(R2=0.999 9,n=9),水杨酸溶液的线性范围为0.2~80μg·m L-1(R2=0.999 9,n=6),水杨酸酰胺溶液的线性范围为0.1~40μg·m L-1(R2=0.999 7,n=6),中间体的线性范围为0.1~50μg·m L-1(R2=0.999 9,n=7);精密度良好,地拉罗司0.1%自身对照溶液重复进样的RSD值为0.35%;分别以水杨酸、水杨酸酰胺和中间体进行回收率试验,平均回收率分别为99.83%(RSD=1.68%),98.26%(RSD=1.47%)和99.24%(RSD=1.58%);分别按杂质对照品外标法和主成分自身对照法计算杂质含量,3批样品最大单个杂质均不超过0.07%,总杂质含量不超过0.23%。结论:本方法准确、灵敏、专属性强,能有效地测定地拉罗司中的有关物质。
Objective: To establish a method for the determination of delaloximab by high performance liquid chromatography (HPLC). Methods: The mobile phase A was consisted of CAPCELL PAK C18MG Ⅱ (250 mm × 4.6 mm, 5 μm), 0.05 mol·L-1 sodium dihydrogen phosphate solution (phosphoric acid adjusted to p H 3.5) and acetonitrile as mobile phase B The detection wavelength was 245 nm and the flow rate was 1.0 m L · min-1. The results showed that there was a good separation between dendrolimus and raw materials, intermediates and other impurity peaks. The range of delallaosil was 0.1-40 μg · m L -1 (R2 = 0.999 9, n = 9) The linear range of salicylamide solution was 0.2 ~ 80μg · m L -1 (R2 = 0.999 9, n = 6). The linear range of salicylamide solution was 0.1-40μg · m L -1 (R2 = 0.999 7, n = 6) The linear range of the intermediate was 0.1-50μg · m L-1 (R2 = 0.999 9, n = 7). The precision was good and the RSD value of 0.1% self-control solution of doraxole was 0.35% The average recoveries of salicylic acid, salicylic acid amide and intermediates were 99.83% (RSD = 1.68%), 98.26% (RSD = 1.47%) and 99.24% (RSD = 1.58% Impurity reference substance standard method and the main component of the self-control method to calculate the impurity content, the three largest single sample impurities are not more than 0.07%, the total impurity content does not exceed 0.23%. Conclusion: The method is accurate, sensitive and specific, which can effectively determine the related substances in dalarocladium.