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目的:建立川芎提取物中HPD-300型大孔吸附树脂残留物的测定方法,为大孔树脂的推广提供参考。方法:选择二甲基亚砜溶解川芎提取物,采用顶空进样方式,运用毛细管气相色谱法测定大孔树脂中有机溶剂的残留量,柱温为程序升温(起始温度50℃,保持10 min;以5℃·min-1的速率升至70℃,保持16 min;以5℃·min-1的速率升至120℃,保持10 min),进样口温度220℃,分流比10∶1,压力58.799 k Pa,总流量10.772 m L·min-1,H2流量40 m L·min-1,空气流量300 m L·min-1,尾吹(N2)流量30 m L·min-1,载气(N2)流量20 m L·min-1。顶空条件为样品温度80℃,阀箱温度100℃,管路温度110℃,平衡时间30 min,进样间隔55 min,进样量1 m L。结果:7种有机溶剂残留物的峰面积与质量浓度呈良好线性关系,相关系数均>0.999,正己烷、环己烷、苯、甲苯、二甲苯、苯乙烯及二乙烯苯的平均回收率分别为99.2%,97.3%,103.4%,98.7%,97.0%,101.9%,98.5%。结论:该方法适用于HPD-300型大孔吸附树脂残留物的测定。
OBJECTIVE: To establish a method for the determination of residues of HPD-300 macroporous adsorption resin in Chuanxiong extract for reference of the promotion of macroporous resin. Methods: Chuanxiong extract was prepared by dimethylsulfoxide (DMSO) solution. Headspace injection was used to determine the residual amount of organic solvent in macroporous resin by capillary gas chromatography. The column temperature was programmed temperature (initial temperature 50 ℃, 10 min; the temperature was raised to 70 ° C at a rate of 5 ° C · min-1 for 16 min; the temperature was raised to 120 ° C at a rate of 5 ° C · min-1 for 10 min; the inlet temperature was 220 ° C; 1, pressure 58.799 k Pa, total flow 10.772 m L · min-1, H2 flow 40 m L · min-1, air flow 300 m L · min-1 and tail gas (N2) flow 30 m L · min -1 , Carrier gas (N2) flow 20 m L · min-1. Headspace conditions were the sample temperature 80 ℃, the valve box temperature 100 ℃, the pipeline temperature 110 ℃, the equilibrium time 30 min, the injection interval 55 min, the injection volume 1 m L. Results: The peak areas and mass concentrations of seven organic solvents showed a good linear relationship with the correlation coefficients> 0.999. The average recoveries of n-hexane, cyclohexane, benzene, toluene, xylene, styrene and divinylbenzene were 99.2%, 97.3%, 103.4%, 98.7%, 97.0%, 101.9%, 98.5%. Conclusion: This method is suitable for the determination of HPD-300 macroporous resin residues.