HPLC-CAD法测定十六烷基二酸单叔丁酯有关物质

Determination of Related Substances in tert-Butyl Hydrogen Hexadecanedioate by HPLC-CAD

目的建立高效液相色谱-电雾式检测器法(HPLC-CAD)测定十六烷基二酸单叔丁酯有关物质。方法以YMC Triart C_(18)4.6×150 mm,3μm为色谱柱,乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,流速1.0 mL·min^(-1);CAD检测器雾化温度Low(35℃),数据采集频率10 Hz。结果十六烷基二酸单叔丁酯、十六烷二酸、十四烷二酸叔丁酯、十五烷二酸叔丁酯、十八烷二酸单叔丁酯和十六烷二酸二叔丁酯分离良好,且均在相应质量浓度范围内,相关系数r均大于0.99,线性关系良好。各杂质的回收率均在80%~120%范围内,RSD(n=9)均小于10%。结论本法操作简便,测定结果准确,重复性好,可用于十六烷基二酸单叔丁酯有关物质的检测,为药品质量的控制提供了重要参考依据。

OBJECTIVE To establish a HPLC-CAD method for determination of related substances in tert-Butyl Hydrogen Hexadecanedioate.METHODS The separation was performed on a YMC Triart C_(18) column(4.6×150 mm,3μm)by gradient elution using 0.1% formic acid-acetonitrile,the flow rate was 1.0 mL·min^(-1).The detector of charged aerosol detector(CAD)was applied with at low nebulization temperature at 35℃ and collection frequency at 10 Hz.RESULTS Under the above chromatographic conditions,this method successfully achieved affable separation among the peaks of tert-Butyl Hydrogen Hexadecanedioate,it's adjacent impurities and the other impurities obtained.Within a certain concentration range,tert-Butyl Hydrogen Hexadecane-dioate,Hexadecanedioic acid,14-(tert-butoxy)-14-oxotetradecanoic acid,15-(tert-butoxy)-15-oxo-pentadecanoic acid,18-(tert-butoxy)-18-oxooctadecanoic acid and di-tert-butyl hexadecan-edioate had good linear respectively.Correlation coefficients r were all greater than 0.99.The recoveries of all known impurities were in the range of 80%-120% with RSD(n=9)less than 10%.CONCLUSION The method is easy to operate,accurate and reproducible,which can be used for the detection of related substances in tert-Butyl Hydrogen Hexade-canedioate.It provides an important reference for drug quality control of drug quality.