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目的建立毛细管气相色谱法测定汉防己甲素中甲醇、乙醇、丙酮、三氯甲烷、苯、环己烷6种有机溶剂的残留量的方法。方法采用Rtx-1毛细管色谱柱(30m×0.25mm,0.25μm),以氮气为载气,FID检测器,以N,N-二甲基甲酰胺(DMF)为溶剂,程序升温,起始温度为30℃,保持7.5min,再以5℃·min-1升至35℃,保持11.5min,最后以40℃·min-1升至200℃,保持10min。结果 6种有机溶剂在各自的浓度范围内具有良好的线性,r为0.9987～0.9999,平均回收率为99.6%～105.9%,最低检测限分别为0.30,0.22,0.16,0.88,0.03和0.10μg·mL-1。结论本方法简便灵敏,结果准确可靠,重复性好,适用于汉防己甲素中有机溶剂残留量的检测。
OBJECTIVE To establish a method for the determination of the residues of 6 kinds of organic solvents of methanol, ethanol, acetone, chloroform, benzene and cyclohexane of tetrandrine by capillary gas chromatography. Methods Rtx-1 capillary column (30m × 0.25mm, 0.25μm), nitrogen as carrier gas, FID detector, N, N-dimethylformamide (DMF) At 30 ℃ for 7.5min, then at 5 ℃ · min-1 to 35 ℃ for 11.5min and finally to 200 ℃ at 40 ℃ · min-1 for 10min. Results Six kinds of organic solvents showed good linearity in the range of their respective concentrations. The average recoveries were from 0.9987 to 0.9999 and the average recoveries were from 99.6% to 105.9%. The lowest detection limits were 0.30, 0.22, 0.16, 0.88, 0.03 and 0.10 μg · mL-1. Conclusion The method is simple and sensitive, accurate, reliable and reproducible. It is suitable for the determination of residual organic solvents in tetrandrine.