顶空气相色谱法测定盐酸伐昔洛韦中的残留溶剂

目的:建立测定盐酸伐昔洛韦中残留溶剂甲醇、乙醇、丙酮和四氢呋喃含量的方法。方法:采用水溶液顶空进样气相色谱法测定3批样品中残留溶剂的含量。色谱柱:Agilent DB-5;柱温:35℃;进样口温度:200℃;火焰离子化检测器温度:260℃;流速:1.5mL·min-1;分流比:1:1;载气:氮气;顶空炉温度:80℃(平衡时间:45min)。按外标法进行定量分析。结果:甲醇、乙醇、丙酮和四氢呋喃具有良好的分离度(均大于4.0),检测浓度线性范围分别为:37.5～750、62.5～1250、62.5～1250、9～180μg·mL-1(r=0.9990～0.9995,n=5),回收率分别为:103.0%(RSD=2.6%)、98.9%(RSD=1.0%)、102.2%(RSD=1.8%)、105.1%(RSD=3.1%)。3批样品中4种溶剂的残留量均小于2010年版《中国药典》对其的规定限度。结论:该方法简单、准确、灵敏度高,能达到残留溶剂的检测要求,可用于盐酸伐昔洛韦中残留溶剂的检测。

Determination of Residual Solvents in Valaciclovir Hydrochloride by Headspace Gas Chromatography

OBJECTIVE:To establish a method for the determination of residual solvents(methanol,ethanol,acetone and tetrahydrofuran) in valaciclovir hydrochloride.METHODS:The contents of residual solvents in 3 batches of samples which were dissolved in water were determined by headspace gas chromatography.The determination condition was as follows:Agilent DB-5 capillary column,column temperature of 35 ℃,injector temperature of 200 ℃,FID detector temperature of 260 ℃,flow rate of 1.5 mL·min-1,split ratio of 1:1,nitrogen as gas carrier,headspace furnace temperature of 80 ℃,equilibrium time of 45 min.Quantitative analysis was conducted according to external standard method.RESULTS:The separation degree of methanol,ethanol,acetone and tetrahydrofuran was well and more than 4.0.The linear ranges of them were 37.5～750 μg·mL-1,62.5～1 250 μg·mL-1,62.5～1 250 μg·mL-1,9～180 μg·mL-1(r=0.999 0～0.999 5,n=5) respectively.Average recoveries were 103.0%(RSD=2.6%),98.9%(RSD=1.0%),102.2%(RSD=1.8%),105.1%(RSD=3.1%).The contents of 4 residual solvents in 3 batches of samples were all lower than the standard stated in Chinese Pharmacopeia(2010 edition).CONCLUSION:The method has been proved to be simple,sensitive and accurate,and it is up to the requirements of residual solvent determination.It can be applicable in the detection of residual solvents in valaciclovir hydrochloride.