顶空-气相色谱法测定葡萄糖氯化钠注射液中12种溶剂残留量  

Determination of 12 solvents residues in glucose sodium chloride injection by headspace-gas chromatography

作　　者：黄祝刚 李亚囡 孙滨滨 贾佳 唐彬 郑琪欣 HUANG Zhugang;LI Yanan;SUN Binbin;JIA Jia;TANG Bin;ZHENG Qixin(Shandong Qidu Pharmaceutical Co.,Ltd.,Zibo 255400,China)

机构地区：[1]山东齐都药业有限公司,山东淄博255400

出　　处：《化学分析计量》2020年第3期68-71,共4页Chemical Analysis And Meterage

摘　　要：建立顶空-气相色谱法测定葡萄糖氯化钠注射液中12种残留溶剂含量的方法。采用HP-INNOWAX毛细管色谱柱(60 m×320μm,0.5μm)为分离柱,检测器为氢火焰离子化检测器(FID),柱温为程序升温。12种残留溶剂乙醇、异丙醇、丙酮、丁酮、乙酸乙酯、乙酸丁酯、乙酸正丙酯、甲苯、乙苯、对二甲苯、邻二甲苯、间二甲苯均能完全分离,在考察的浓度范围内线性关系良好(r>0.995),检出限分别为0.055,0.019,0.023,0.070,0.155,0.013,0.003,0.009,0.004,0.004,0.004,0.005μg/mL。平均回收率为90.6%~109.0%,测定结果的相对标准偏差为2.2%~5.6%(n=9)。该方法专属性强,精密度、准确度和检测灵敏度高,重复性好,可用于葡萄糖氯化钠注射液中12种溶剂残留量的测定。The method for the determination of 12 residual solvents in glucose and sodium chloride injection by headspace-gas chromatography was developed.HP-INNOWAX capillary column(60 m×320μm,0.5μm)and hydrogen flame ionization detector(FID)were used for determination by programmed temperature rise.The 12 kinds of residual solvents(ethanol,isopropanol,acetone,butanone,ethyl acetate,butyl acetate,normal propyl acetate,toluene,ethyl benzene and p-xylene,o-xylene,m-xylene)were completely separated,and the linear relationship was good within the concentration range(r>0.995),and the detection limits were 0.055,0.019,0.023,0.070,0.155,0.013,0.003,0.009,0.004,0.004,0.004,0.005μg/mL,respectively.The recovery was 90.6%-109.0%,and the relative standard deviation was 2.2%-5.6%(n=9).The method has strong specificity with high precision,accuracy,detection sensitivity and good repeatability,which can be used for the determination of 12 residual solvent residues in glucose and sodium chloride injection.

关 键 词：顶空-气相色谱法 葡萄糖氯化钠注射液 残留溶剂 

分 类 号：O657.7[理学—分析化学]