顶空气相色谱法测定眼氨肽制剂中乙醇残留量  

Determination of ethanol residue in ocular extractives preparations by headspace gas chromatography

作　　者：覃婷婷 伏圣青 黄哲甦 Qin Tingting;Fu Shengqing;Huang Zhesu(Tianjin Institute for Drug Control,Tianjin 300070)

机构地区：[1]天津市药品检验研究院,天津300070

出　　处：《天津药学》2020年第2期14-16,共3页Tianjin Pharmacy

摘　　要：目的:建立测定眼氨肽制剂中乙醇残留量的方法。方法:采用顶空气相色谱法,色谱柱为CP-WAX 52 CB FS(50 m×0.32 mm,5μm),程序升温,进样口温度为200℃,检测温度为220℃,检测器为氢火焰离子化检测器(FID),载气为氮气,载气流速为1.5 ml/min,分流比为20:1,顶空平衡温度为85℃,顶空平衡时间为20 min,顶空进样量为1 ml。结果:乙醇线性范围为0.4~303.4μg/ml,线性方程为Y=0.0054X-0.0057(r=0.9999);检测限为0.1μg/ml,定量限为0.4μg/ml;重复性试验RSD为0.53%;平均回收率为100.28%(RSD为1.80%,n=9)。结论:该方法操作简便、准确,精密度高、重复性好,可用于眼氨肽制剂中乙醇残留量的测定。Objective:To establish a method for the determination of ethanol residues in Ocular Extractives preparations.Methods:Headspace gas chromatography was used and the parameters were optimized.The column was CP-WAX 52 CB FS(50 m×0.32 mm,5μm).The temperature was programmed,the inlet temperature was 200℃,and the detection temperature was220℃.The detector was hydrogen flame ionization detector(FID),and the carrier gas was nitrogen(flow rate 1.5 ml/min,split ratio 20:1).The headspace equilibrium temperature was 85℃,the headspace equilibration time was 20 minutes,and the headspace injection volume was 1 ml.Results:The linear range of ethanol was 0.4~303.4μg/ml,and the linear equation was Y=0.0054 X-0.0057(r=0.9999).The detection limit was 1μg/ml,and the limit of quantification was 4μg/ml.The repeatability test RSD was 0.53%,and the sample recovery was 100.28%(RSD=1.80%,n=9).Conclusion:A simple,accurate,high precision and repeatable method was established for the determination of ethanol residues in Ocular Extractives preparations.

关 键 词：眼氨肽制剂 顶空气相色谱法 乙醇残留量 

分 类 号：R927.2[医药卫生—药学]