顶空毛细管气相色谱法测定药用辅料羧甲基淀粉钠中的溶剂残留量

Content Determination of Residual Organic Solvents in Pharmaceutical Excipients Carbonyl Methyl Starch by Headspace Capillary Gas Chromatography

目的:建立顶空气相色谱法测定药用辅料羧甲基淀粉钠中乙醇、异丙醇残留量的方法。方法:采用顶空气相色谱法,以水为溶解介质,色谱柱为DB-1301石英毛细管柱,柱温80℃,检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为150℃。结果:乙醇、异丙醇的检测浓度的线性范围分别为0.025～2.0mg·mL-1(r=0.9999)和0.025～2.0mg·mL-1(r=0.9999);平均回收率分别为99.5%(RSD=0.9%)和99.2%(RSD=1.2%);定量限分别为4.85、2.95μg·mL-1;3批样品中乙醇和异丙醇残留量均符合《中国药典》要求。结论:本方法简单、准确、灵敏度高、重复性好,可用于羧甲基淀粉钠中有机溶剂残留量的测定。

OBJECTIVE： To establish the headspace capillary GC method for the content determination of residual organic solvents （alcohol and isopropyl alcohol） in pharmaceutical excipients carbonyl methyl starch. METHODS： The residual organic solvents were separated on DB-1301 capillary column by headspace GC. The samples were dissolved in water. FID detector was adopted and the column temperature was 80 %. The detector temperature was 250 %. The inlet temperature was 150 %. RESULTS： The linear ranges of alcohol and isopropyl alcohol were 0.025-2.0 mg·mL^-1 （r=0.999 9） and 0.025-2.0 mg·mL^-1 （r=0.999 9）, respectively; the average recoveries were 99.5% （RSD=0.9%） and 99.2% （RSD= 1.2%）; the determination limits were 4.85 μg· mL^-1 and 2.95 μg·mL^-1. 2 kinds of residual organic solvents in 3 batches of samples were all up to the standard stated in Chinese Pharmacopeia. CONCLUSION： The method is simple, accurate, sensitive and reproducible, and it can be used for the content determination of the residual organic solvents in carbonyl methyl starch.