顶空进样－气相色谱法测定盐酸沙格雷酯原料药中有机溶剂残留

采用顶空进样毛细管柱气相色谱法，建立了一种盐酸沙格雷酯原料药中残留溶剂的测定方法。色谱条件：色谱柱为DB－WAX毛细管柱，程序升温方式，氢火焰离子化（FID）检测器，外标法定量。实验结果表明，乙醇、四氢呋喃、异丙醚、乙酸乙酯和丁酮均能得到良好的分离，溶剂对测定无影响，在测试浓度范围内，峰面积与浓度线性关系良好（R2＞0.998），进样精密度实验的RSD值均小于5.0％，乙醇、四氢呋喃、异丙醚、乙酸乙酯和丁酮最低检测限分别为5.00、1.00、0.10、2.00、2.50 m g／L ，加标回收率在97％‐105％之间。方法简单、准确、灵敏度高，重现性好，适用于盐酸沙格雷酯原料药中有机溶剂残留的测定。

Determination of residul organic solvents in sarpogrelate hydrochloride raw material medicine by head- space gas chromatography

A headspace gas chromatography with capillary column method was established for determi‐ning residual organic solvents in the raw material of sarpogrelate hydrochloride .The determination was carried out by the DB‐WAX capillary column with temperature programming and hydrogen flame ionization detector（FID） ,and external standard method for quantitative .The results showed that the residual sol‐vents such as ethanol ,tetrahydrofuran ,isopropyl ether ,ethyl acetate and butanone obtained a good sepa‐ration ,and the solvent had no effect on the determination .The calibration curve of each solvent showed a good linear relationship between the peak area and concentration （R2 ＆gt; 0.998） in the test concentration range ,and the RSD values were less than 5% .The minimun detection limit of ethanol ,tetrahydrofuran , isopropyl ether ,ethyl acetate and butanone were 5.00 ,1.00 ,0.10 ,2.00 ,and 2.50 mg/L respectively . The recovery rate of standard addition was between 97%‐105% .This method is simple ,accurate ,high sensitivity ,good reproducibility ,and is suitable for the determination of residual organic solvents in the raw material of sarpogrelate hydrochloride .