建立美托拉腙中异丙醇、乙醇、1,4-二氧六环和正丁醇4种有机溶剂残留量的气相色谱测定方法.用PEG-20M毛细管色谱柱(0.53 mm×30 m),采取程序控制柱温升温,在27.75 min内柱温从40 ℃经90 ℃升至180 ℃.采用FID检测器,检测器温度为250 ℃,进样口温度为145 ℃;氮气为载气,流速1.5 mL·min-1;氢气流速为35 mL·min-1,空气流速为350 mL·min-1,尾吹气流速为46 mL·min-1,四种有机溶剂完全分离.所得4种溶剂的线性回归方程证实了峰面积与浓度呈良好的线性关系,其相关系数在0.999 3至0.999 8之间.测定了方法的检出限(S/N=3)依次为0.25,5.89,1.66,2.47 mg·L-1,方法的测定限(S/N=10)依次为17.57,10.99,8.51,6.11 mg·L-1,回收率试验的结果在97.9%~101.5%之间.

Four residual organic solvents,i.e.iso-propanol,ethanol,1,4-dioxane and n-butanol in the drug metolazone were determined by gas chromatography,with PEG-20M capillary column (30 m×0.53 mm) and FID detector under programmed column temperature control,raising from 40 ℃ through 90 ℃ to 180 ℃ within 27.75 min.Temperature at the detector was 250 ℃ and at the sample injector was 145 ℃.Nitrogen was used as the carrier gas with flow-rate of 1.5 mL·min-1.Flow-rates used for hydrogen,air and make-up gas were 35,350 and 46 mL·min-1 respectively.The external standard method was used in the determination.Under the specified analytical conditions,the 4 solvents mentioned above were separated quantitatively.Linear relationships between the peak areas and concentrations of the 4 solvents were obtained as shown by their linear regression equations with correlation coefficients in the range of 0.999 3-0.999 8.Values of detection limits (S/N=3) and determination limits (S/N=10) of the method found were 0.25,5.89,1.66,2.47 mg·L-1 and 17.57,10.99,8.51,6.11 mg·L-1 for iso-propanol,ethanol,1,4-dioxane and n-butanol respectively.Results of recovery test obtained were in the range of 97.9%-101.5%.