顶空气相色谱法测定聚桂醇中环氧乙烷和二氧六环的含量 |
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引用本文: | 王发,徐春燕,王嫦鹤,张秉华,王涛.顶空气相色谱法测定聚桂醇中环氧乙烷和二氧六环的含量[J].安徽医药,2013,17(1):33-34. |
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作者姓名: | 王发 徐春燕 王嫦鹤 张秉华 王涛 |
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作者单位: | 陕西省食品药品检验所,陕西,西安,710061;陕西天宇制药有限公司,陕西,西安,710075 |
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摘 要: | 目的建立聚桂醇原料药中环氧乙烷和二氧六环的顶空气相色谱测定法。方法以水为溶剂,采用顶空气相色谱法测定,平衡温度100℃,平衡时间40 min。使用DB-1(30 m×0.32 mm×0.25μm)毛细管柱,检测器为FID,进样口温度150℃,检测器温度250℃。程序升温,初温35℃,10 min,30℃.min-1至230℃,10 min。结果环氧乙烷在1.01~10.14mg·L-1质量浓度范围内与峰面积呈良好的线性关系Y=1.044 0X+1.159 8(r=0.999 2),回收率为102.6%,RSD为2.3%(n=9)。二氧六环在4.98~49.8mg·L-1质量浓度范围内与峰面积呈良好的线性关系Y=0.410 5X-0.915 6(r=0.999 7),回收率为101.8%,RSD为2.9%(n=9)。结论该方法准确可靠,能有效控制聚桂醇原料的质量。
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关 键 词: | 顶空进样 气相色谱法 聚桂醇 环氧乙烷 二氧六环 |
Head-space capillary GC for the determination of ethylene oxide and dioxane in lauromacrogol |
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Institution: | WANG Fa1,XU Chun-yan2,WANG Chang-he1,et al(1.Shaanxi Province Institute for food and Drug Control,Xian,Shaanxi 710061,China; 2.Shaanxi Tianyu Pharmaceutical Co.Ltd,Xian,Shaanxi 710075,China) |
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Abstract: | Objective To establish a headspace capillary GC method for the determination of ethylene oxide and dioxane in lauromacrogol.Methods The samples were injected by headspace while water was used as solvent.DB-1(30 m×0.32 mm×0.25 μm) was used.The inlet temperature was 150℃ and the FID detector temperature was 250 ℃.The oven temperature was initially held at 35℃ for 10 min and was then programmed to 230℃ at 30℃·min-1and held for 10 min.Results The linearity equation of ethylene oxide was Y =1.044 0X+1.159 8(r=0.999 2),the average recovery was 102.6%(n=9,RSD =2.3%),and the linear range was 1.01~10.14 mg·L-1.The linearity equation of dioxane was Y =0.410 5X-0.915 6(r=0.999 7),the average recovery was 101.8%(n=9,RSD =2.9%),and the linear range was 4.98~49.8 mg·L-1.Conclusion The method is rapid and accurate,so it is proposed for the quality control of lauromacrogol. |
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Keywords: | head-space injecting GC iauromacrogol ethylene oxide dioxane |
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