论文部分内容阅读
目的:测定辛伐他汀中残留有机溶剂甲醇、乙醇、环己烷、甲苯和N,N-二甲基甲酰胺的含量。方法:采用气相色谱法,氢火焰离子化检测器(FID),以二甲基亚砜为溶剂,正丙醇为内标,采用石英毛细管柱DB-624(0.32 mm×30m,1.8μm),以6％氰丙基苯-94％二甲基硅氧烷为固定相,柱温115℃维持8 min,以30℃·min~(-1)的速率升温至180℃,维持4min,气化室温度:200℃;检测器温度:240℃(FID);载气:氮气;分流比:1:60;柱前压:30 kPa;尾吹:50 mL·min~(-1);灵敏度:1;衰减4。实现了各组分的基线分离。结果:3批样品中5种有机溶剂残留量均符合要求。结论:经方法学试验验证,该方法灵敏、准确、可靠,适用于本品有机溶剂残留量的测定。
OBJECTIVE: To determine the content of residual organic solvents methanol, ethanol, cyclohexane, toluene and N, N-dimethylformamide in simvastatin. Methods: Gas chromatography, flame ionization detector (FID), dimethylsulfoxide (DMSO) and n-propanol were used as internal standards. With 6% cyanopropylbenzene-94% dimethylsiloxane as the stationary phase, the column temperature was maintained at 115 ℃ for 8 min and the temperature was raised to 180 ℃ at the rate of 30 ℃ · min ~ (-1) Room temperature: 200 ℃; Detector temperature: 240 ℃ (FID); Carrier gas: Nitrogen; Split ratio: 1: 60; 1; attenuation 4. Baseline separation of the components was achieved. Results: The residues of the five organic solvents in the three batches of samples all met the requirements. Conclusion: The method validation, the method is sensitive, accurate and reliable, suitable for the determination of residual organic solvents.