顶空进样气相色谱法测定脑脉通软胶囊中有机溶剂残留量

Determination of residual solvents in Naomaitong soft capsule by headspace GC

关键词:  气相色谱法  有机溶剂残留量  大孔吸附树脂  脑脉通

Key words:  GC  residues of organic solvent  macroporous resin  Naomaitong

摘要:

[目的]建立测定脑脉通软胶囊中有机溶剂残留量的方法,为质量评价提供依据。[方法]采用顶空进样气相色谱法,以50%二甲基甲酰胺水溶液为提取溶剂,色谱柱为DB-624石英毛细管柱,75 m×0.530 mm,df=3.00μm;FID检测器温度为250℃;氮气为载气,流速15 mL/min,恒流方式;程序升温,起始温度50℃维持18 min,以100℃/min升温速率升至80℃,再以2℃/min的升温速率升至112℃,再以100℃/min的升温速率升至160℃,维持10 min,再以100℃/min的升温速率升至200℃,维持5 min;气化室温度为250℃;顶空瓶温度90℃,顶空时间40 min,进样时间1 min。[结果]脑脉通软胶囊中各残留溶剂均未检出,6种溶剂在0～40μg/mL的浓度范围内线性关系良好,最小检测限为0.2～2.8μg/mL;精密度RSD小于5.6%(n=5),平均回收率为18.8%～48.3%(RSD为5.1%～6.4%,n=5),所以采用标准加入法进行测定计算;对照品溶液中各成分24 h之内均稳定(RSD为0.5%~8.9%,n=5)。[结论]所建立的方法准确、快速、灵敏,该方法能够控制脑脉通软胶囊中有机溶剂残留量。

Abstract:

[Objective] To establish the method for analysis on organic solvent residues in Naomaitong soft capsule in order to provide the basis for quality assessment.[Methods] GC instrument coupled with headspace sampler was used and taking 50% of the aqueous solution of dimethylformamide as the solvent.The column was DB-624 capillary column(75 m×0.530 mm,df=3.00 μm);FID detector temperature was 250 ℃;A nitrogen flow rate was set at 15 mL/min in a constant flow mode;Oven temperature program was used from 50 ℃(18 min) to 80 ℃ at a rate of 100 ℃/min,then to 112 ℃ at a rate of 2 ℃/min,next to 160 ℃(10 min) at a rate of 100 ℃/min,finally to 200 ℃(5 min)at a rate of 100 ℃/min;Gasification chamber temperature was 250 ℃.The headspace vials were balanced at 90 ℃ for 40 min,the injection time was 1 min.[Results] The residual solvents were not detected in Naomaitong soft capsule.A good linear behavior was found in the concentration ranging from 0 to 40 μg/mL.The LODs were 0.2～2.8 μg/ml,the precisions RSD were less than 5.6%(n=5).The average recoveries were in the range from 18.8% to 48.3%,with RSD of 0.5%~8.9%(n=5).The components of reference solution were stable within 24 h(RSD,0.5%~8.9%,n=5).[Conclusion] The method is accurate,rapid and sensitive,so it can be used for controlling the organic residual solvents of Naomaitong.