顶空气相色谱法测定盐酸帕洛诺司琼中的11种残留溶剂

Determination of the 11 residual solvents in Palonosetron hydrochloride by Headspace GC

目的采用顶空毛细管气相色谱法测定盐酸帕洛诺司琼中11种残留溶剂的残留量。方法采用DB-624毛细管色谱柱(30 m×0. 32 mm,1. 8μm),二甲亚砜为溶解介质,FID检测器,进样口温度200℃,检测器温度250℃;载气为氮气,流速2 m L·min^(-1);柱温初始温度为35℃,维持11 min,以40℃·min^(-1)升温至200℃,维持3 min;分流比为5∶1。结果各组分在所考察的浓度范围内均呈良好的线性关系;甲醇、乙醇、异丙醇、乙酸乙酯、乙醚、正己烷、三氯甲烷、四氢呋喃、甲苯、二甲基甲酰胺、二氯甲烷的平均加样回收率分别为98. 1%、96. 5%、95. 6%、92. 8%、94. 0%、98. 4%、84. 6%、93. 9%、83. 1%、94. 5%、89. 6%;各组分的最低检出浓度分别为3. 6037、2. 7984、1. 7883、0. 7435、0. 0186、0. 0189、0. 1494、0. 0692、0. 0035、2. 6288、0. 0742μg·g^(-1)。结论所用方法快速、灵敏、准确,适用于盐酸帕洛诺司琼中残留溶剂的检查。

OBJECTIVE To establish a headspace GC method for the simultaneous determination of eleven kinds of residual solvents in Palonosetron hydrochloride.METHODS Headspace GC with DB-624 column(30 m×0.32 mm,1.8μm),the solvent medium was dimethyl sulfoxide and the detector was FID.The injector temperature was 200℃with the detector temperature of 250℃and the carrier gas of nitrogen.The flow rate is 2 m L·min^-1.The column temperature changed according to the program:maintaining the temperature of the column at 35℃for 11 min,then raising the temperature at a rate of 40℃per min to 200℃,and maintaining in for 3 min.The split ratio was 5∶1.RESULTS The results showed good linearity.The sample recovery of methanol,ethanol,2-propanol,ethyl acetate,ethyl ether,hexane,chloroform,tetrahydrofuran,toluene,N,N-dimethylformamide,and dichloromethane was 98.1%,96.5%,95.6%,92.8%,94.0%,98.4%,84.6%,93.9%,83.1%,94.5%and 89.6%,respectively.The minimum detection concentrations was 3.6037,2.7984,1.7883,0.7435,0.0186,0.0189,0.1494,0.0692,0.0035,2.6288,0.0742μg·g^-1.The results showed good precision.CONCLUSION The method is simple,sensitive and accurate,and suitable for the determination of residual solvents in Palonosetron hydrochloride.