HPLC法同时测定雷贝拉唑钠原料药中8个有机杂质的含量

Simultaneous determination of eight organic impuritiesin drug substance of rabeprazole sodium by HPLC method

利用高效液相色谱（HPLC）技术建立了一种同时测定雷贝拉唑钠原料药中8个有机杂质的新方法。该方法采用二元高压梯度洗脱方式，以pH=6．0的磷酸盐缓冲溶液（A）-乙腈（B）为流动相，进行梯度洗脱（0-10min，85％A→65％A；10-35min，60％A；35-35．01min，60％A→85％A；35．01-40min，85％A），流速为1mL／min，以YMC Triart C18柱为分离柱，柱温为30℃；采用紫外检测器，检测波长为285nm。研究结果表明，各已知杂质、主成分之间均能彼此分离，空白溶剂对各杂质的测定无干扰，各已知杂质的峰面积与浓度呈良好的线性关系，相关系数均大于0．990，各已知杂质的平均回收率均在83．2％-115．9％范围内，RSD为1.1％-4．3％。该方法简便有效，适用于雷贝拉唑钠原料药的质量控制，具有很高的灵敏度和准确度。

A novel HPLC method was developed for simultaneous determination of eight organic impurities in drug substance of rabeprazole sodium. Abinary high pressure gradient elution mode was employed, and the mobile phase consisted of phosphate buffer at pH6.0 （A） and acetonitrile （B）. The proportion of A to B （V/V） in the mobile phase was 85 to 15 at the start of each run, ramped to 60 to 40 at 10 min and held until 35 rain, then returned to 85 to 15 at 35.01 rain and held until 45 rain recondition the column. The flow rate was 1 mL/min.A YMCTriart C18 column at 30 ℃ and a UV detector at 285 nm were used. Each specified impurity and rabeprazole sodium can be separated from each other, and the blank solvent does not interfere with the test of each impurity. In this method the peak areas of each impurity versus its concentrations over the investigated range have good linearity, and the correlation coefficients （R） are all more than 0.990. The average recoveries of each specified impurity are all in the range of 83. 2% to 115.9%, with RSDs from 1.1% to 4. 3%. The proposed method is simple, convenient and efficient, which can be used for the quality control of rabeprazole sodium with high sensitivity and accuracy.