GC 法测定盐酸法舒地尔中有机溶剂残留量

目的建立GC法测定盐酸法舒地尔中有机溶剂残留量。方法采用GC法，FID检测器；进样口温度160℃；柱温为60℃；检测器温度280℃；尾吹30ml·min^-1，进样量1μl。结果乙醇浓度在20．736～1036．8μg·ml^-1，二氯甲烷浓度在5．04—126μg·ml^-1，N，N-二甲基甲酰胺浓度在6．48—162μg·ml^-1的范围内，浓度与峰面积有良好的线性关系，r值在0．9994以上；最低检测限分别为2．10、1．21、2．74ng；平均回收率为乙醇99．23％，二氯甲烷100．23％，N，N-二甲基甲酰胺100．24％，RSD分别为1．46％，2．87％，1．92％（n=9）。结论本方法准确，方便，灵敏，适用于盐酸法舒地尔中有机残留量的检测。

Determination of Residual Organic Solvents in Fasudil Hydrochloric via GC Method

Objective To establish a method for determining the residual organic solvents in fasudil hydro-chloric using gas chromatography. Methods The residual solvents were determined by GC and the FID detector was adopted. The atmosphere was nitrogen ,the entrance temperature of the column was 160 ℃, the column temperature was 60 ℃, the tail blowing was 30 ml·min^-1, and the sample size was 1 μl. Results The concentration of alcohol, methylene chloride and N, N-Dimethylformamide ranged from 20. 736 μg·ml^-1 to 1036.8 μg ·ml^-1,5.04 μg ·ml^-1 to 126 μg ·ml^-1 ,and 6.48 to 162 μg ·ml^-1 ,respectively. There was a good linear relation between the three con-centrations and the peak areas. All the correlation coefficients were above 0. 9994. The limit of detection was 2.10, 1.21,2.74 ng, the average recovery was 99.23%, 100.23%, 100.24%, and the RSD was 1.46% ,2.87%, 1.92% （ n =9）, respectively. Conclusion This method is accurate,simple and sensitive. It can be used for deter- mining residual organic solvents in hydrochloric fasudil.