HPLC-MS法测定甲磺酸多拉司琼原料药中有关物质和异构体含量

Content Determination of the Related Substances and Isomeride in Dolasetron Mesylate Raw Material by HPLC-MS

目的:建立甲磺酸多拉司琼原料药中有关物质和异构体含量测定的方法。方法:采用高效液相色谱-质谱法测定3批甲磺酸多拉司琼原料药中的有关物质和异构体含量。色谱柱为shim-packVP-ODS;流动相A为0.01mol·L-1甲酸铵溶液(用三乙胺调m节inp-H1;至检7测.0)波-乙长腈为(29150∶5n)m,。流质动谱相条B件为采0.0用1电mo喷l.雾L-电1甲离酸源铵(E溶S液I)(、正用离三子乙检胺测调节模式pH。至结7果.0):-有乙效腈(分2离7∶了73)甲,磺梯酸度多洗拉脱司,流琼速与为有1关.0物mL质.及异构体(R>1.5),甲磺酸多拉司琼的最低检测限为0.5ng,3批样品中单个杂质含量≤0.05%,总杂质含量<0.1%,异构体未检出。结论:本方法准确、专属性好,适用于甲磺酸多拉司琼原料药中有关物质和异构体的检测。

OBJECTIVE：To establish a method for the content determination of the related substances and isomeride in dolasetron mesylate raw material. METHODS：HPLC-MS method was adopted to determine the contents of the related substances and isomeride in 3 batches of dolasetron mesylate raw material. The separation was performed on shim-pack VP-ODS column with mobile phase A consisted of 0.01 mol·L^-1 ammonium formate solution （pH value adjusted to 7.0 with triethylamine）-acetonitrile（95 ： 5） and mobile phase B consisted of 0.01 mol·L^-1 ammonium formate solution （pH value adjusted to 7.0 with triethylamine）-acetonitrile （27：73）at the flow rate of 1.0 mL·min^-1（gradient elution）. The detection wavelength was set at 210 nm. Electrospray ionization （ESI） source was applied and operated in positive mode. RESULTS： Related substance and isomeride were separated from dolasetron mesylate effectively （R〉1.5）. The lowest detection limit of dolasetron mesylate was 0.5 ng. The content of single impurity in 3 batches of samples was no more than 0.05% and total content of impurity was lower than 0.1%. Isomeride was not found. CONCLUSIONS：The method is accurate and specific, and it can be used for the determination of the related substances and isomeride in dolasetron mesylate raw material.