毛细管气相色谱法测定羟丙基-β-环糊精中的有机溶剂残留量

Determination of Residual Organic Solvents in Hydroxypropyl-β-cyclodextrin by Capillary Gas Chromatography

目的:建立毛细管气相色谱法测定羟丙基-β-环糊精中乙醇和1,2-丙二醇的残留量的方法。方法:色谱柱为DB-624石英毛细管柱,柱温采用程序升温,FID检测器,检测器温度为250℃,进样口温度为250℃,以二甲亚砜为溶剂。结果:乙醇、1,2-丙二醇的检测浓度的线性范围分别为0.1～5.0 mg·ml^(-1)(r=0.999 9)、0.1～5.0 mg·ml^(-1)(r=0.999 7);平均回收率为分别为99.0%,98.2%,(RSD分别为1.9%,2.2%);最低检出限分别为1.03,0.81 ng;3批样品中2种有机溶剂残留量均符合《中国药典》要求。结论:本方法简单、准确、灵敏度高、重复性好,可用于该药物中有机溶剂残留量的测定。

Objective： To establish a capillary GC method for the determination of residual organic solvents-alcohol and 1,2-Pro- panediol in hydroxypropyl-β-cyelodextrin. Method： The residual organic solvents were separated on DB-624 capillary column using temperature programming. FID was used as detector with a temperature of 250 ℃ ,the inlet temperature was 2：50 ℃, and DMSO as the solvent. Result： The linear ranges of alcohol and 1,2-propanediol were 0.1-5.0 mg·ml^- 1 （ r = 0.999 9） and 0.1-5.0 mg·ml^- 1 （ r = 0. 999 7） ,respectively. The average recoveries were 98.2% and 99.0% with RSD 1.9% and 2.2% , respectively. The detection limits were 1.03 ng and 0.81 ng, respectively. The residual levels for the two organic solvents in 3 batches samples were all up to the standard stipulated in china pharmacopeia. Conclusion： The method is simple, accurate, sensitive and reproducible, it can be used for the deter- mination of the residual organic solvents in hydroxypropyl-β-eyelodextrin.