GC法测定盐酸乙胺丁醇原料中残留溶剂的含量

Determination of residual solvents in material drug of ethambutol hydrochloride by gas chromatography

目的建立测定盐酸乙胺丁醇原料中残留溶剂含量的方法。方法气相色谱法与顶空进样法。色谱柱为DB-624毛细管柱,柱温为50℃,进样口温度为150℃；检测器为FID,温度为200℃；载气为氮气,流速为32 KP；进样量100μL。结果结果表现出了良好的线性关系,甲醇、异丙醇、1,2-二氯乙烷、环己烷检测浓度线性范围分别为2.5～20 mg·L-1（r=0.998 5）、250～1 000 mg·L-1（r=0.998 1）、0.25～2 mg·L-1（r=0.995 3）、2.5～20 mg·L-1（r=0.996 2）,平均回收率分别为101.54%、103.66%、103.07%、99.17%,RSD分别为2.1%、1.8%、4.4%、3.8%,最低检测限分别为0.5、25、0.05、0.5 mg·L-1。结论建立的方法简便、灵敏、准确,适用于盐酸乙胺丁醇原料的残留溶剂含量的测定。

Objective To establish a GC method for the determination of residual solvents in material drug of ethambutol hydrochloride. Methods GC and headspace sample injection method were adopted. The determination was performed with a DB-624 capillary column（column temperature was 50 ℃） using nitrogen gas as carrier gas at the flow rate of 32 KP and FID as detector. The injector temperature and detector temperature were controlled at 150 ℃ and 200 ℃,respectively. The sample volume was 100 μL. Results The results showed excellent linearity. The linear ranges of residual solvents of methanol,isopropanol,1,2-dichoroethane and cyclohexane were 2. 5 ～ 20 mg·L-1（r =0. 998 5）,250 ～1 000 mg·L-1（r = 0. 998 1）,0. 25 ～ 2 mg·L-1（r = 0. 995 3）,2. 5 ～ 20 mg·L-1（r = 0. 996 2）,respectively. And their recoveries were 101. 54%,103. 66%,103. 07% and 99. 17%,respectively. RSDs were 2. 1%, 1. 8%,4. 4% and 3. 8%,respectively. The minimum detection limits were 0. 5,25,0. 05 and 0. 5 mg·L-1,respectively. Conclusions The method is simple,sensitive and accurate,which is suitable for content determination of residual solvents in ethambutol hydrochloride.