气相色谱法测定注射用辛芍冻干粉针有机溶剂残留量  

Determination of Residue Organic Solvents in Xinshao Freeze-dried Powder Injection by Gas Chromatography

作　　者：杨先炯[1] 王永林[1] 王爱民[1] 兰燕宇[1] 李勇军[1] 何迅[1] 

机构地区：[1]贵阳医学院,贵州贵阳550004

出　　处：《时珍国医国药》2009年第2期342-343,共2页Lishizhen Medicine and Materia Medica Research

基　　金：贵州省中药现代化科技产业资助项目[No.黔科合农字(2005)500102号]

摘　　要：目的建立以气相色谱法测定注射用辛芍冻干粉针中的有机溶剂乙醇、正丁醇残留量的方法。方法采用内标法顶空进样，以FFAP毛细管柱（30m×0．53mm，lIxm）为色谱柱，柱温为60℃，载气为氮气，柱前压20kPa，进样13＇温度为220℃，FID检测器，检测器温度为250℃，空气流速500ml·min，氢气流速50ml·min-1。结果乙醇、正丁醇分别在2．5～240μg·ml-1（r=0．9996），0．5～48μg·ml-1（r=0．9999）的浓度范围内呈良好的线性关系。平均回收率分别为乙醇100．6％（RSD=2．7％），正丁醇102．2％（RSD=3．3％）。结论该方法重复性好，定量准确，便于操作。Objective To determine the contents of the residual solvents including ethanol and n - butanol in Xinshao Freeze - dried Powder Injection by GC. Methods With Head -space injection, FFAP capillary column（ 30 m × 0.53 mm, 1μ m）was used at 60℃. Nitrogen was used as carrier gas , the column inlet pressure was 20 kPa. The temperature at the injection port and the FID detector were 220℃ and 250℃, respectively. The flow rate of air and hydrogen was 500 ml· min -1 and 50 ml · min-1. Resuits Ethanol, n - butanol showed a good linear relationship over the range of 2.5 - 240 μg·ml-1 （ r = 0.999 6 ） and 0.5 - 48 μg·ml-1（ r = 0. 999 9,with a mean recovery of ethanol 100.6% （RSD = 2.7% ） , n -butanol 102.2% （RSD = 3.3% ） respectively. Conclusion The method is reproducible, precise and simple.

关 键 词：气相色谱 注射用辛芍冻干粉针 残留溶剂 乙醇 正丁醇 

分 类 号：R284.1[医药卫生—中药学]