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    顶空固相微萃取-气相色谱法测定匹伐他汀钙原料药中6种溶剂残留

    Determination of Six Kinds of Residual Solvents in Pitavastatin Calcium by Headspace Solid Phase Microextraction Combined with Gas Chromatography

    • 摘要: 将样品用N,N-二甲基甲酰胺溶解配制成100 g·L-1的样品溶液,取样品溶液10 mL置于顶空瓶中,于40℃水浴加热5 min后,进行固相微萃取,采用聚二甲基硅氧烷萃取头,萃取温度为40℃,吸附时间和脱附时间分别为30,10 s。甲醇、四氢呋喃、乙酸乙酯、乙醇、乙腈、甲苯在SE-54毛细管色谱柱上分离,采用火焰离子化检测器。上述6种溶剂的峰面积与其质量浓度在一定范围内呈线性关系,检出限(3S/N)在1.0~2.3 mg·L-1之间。加标回收率在95.8%~104%之间,测定值的相对标准偏差(n=8)小于9.0%。

       

      Abstract: The sample was dissolved with N,N-dimethylformamide to prepare a sample solution of 100 g·L-1. The sample solution (10 mL) was taken into a headspace vial and heated in a water bath at 40℃ for 5 min. Then solid-phase microextraction was carried out at 40℃ using polydimethylsiloxane extraction head, with adsorption time and desorption time of 30, 10 s, respectively. Methanol, tetrahydrofuran, ethyl acetate, ethanol, acetonitrile, and toluene were separated on a SE-54 capillary column and detected using a flame ionization detector. Linear relationships were found between peak areas and mass concentrations of the above six solvents within definite ranges, with detection limits (3S/N) in the range of 1.0-2.3 mg·L-1. Values of recovery obtained by standard addition method ranged from 95.8% to 104%, and RSDs (n=8) were less than 9.0%.

       

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