GC测定汉防己甲素中的6种残留有机溶剂

Determination of 6 Kinds of Residual Organic Solvents in Tetrandrine by GC

关键词:  气相色谱  汉防己甲素  残留有机溶剂  测定

Key words:  GC  tetrandrine  residual organic solvent  determination

摘要:

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(30 m×0.25 mm，0.25 μm)，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7.5 min，再以5 ℃·min^-1升至35 ℃，保持11.5 min，最后以40 ℃·min^-1升至200 ℃，保持10 min。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0.998 7~0.999 9，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0.10 μg·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。

Abstract:

OBJECTIVE To establish a capillary gas chromatography method for determination of six residual organic solvents including methanol, ethanol, acetone, trichloromethane, benzene and cyclohexane in tetrandrine. METHODS The determination was performed on a Rtx-1 capillary column(30 m×0.25 mm, 0.25 μm) with nitrogen gas as carrier and FID as detector. DMF was used as solvents. The initial column temperature was 30 ℃, maintaining for 7.5 min, then raising the temperature to 35 ℃ at the rate of 5 ℃·min^-1 and maintaining for 11.5 min, then raising the temperature to 200 ℃ at the rate of 40 ℃·min^-1 and maintaining for 10 min. RESULTS The six residual solvents showed good linearity (r=0.998 7-0.999 9) in the experimental concentration ranges. The average recovery rates of the preparation were in the range of 99.6%-105.9%. The detection limits were 0.30, 0.22, 0.16, 0.88, 0.03, 0.10 μg·mL^-1. CONCLUSION The method is simple, sensitive, accurate, and suitable for the determination of the residual organic solvents in tetrandrine.