顶空-气相色谱法测定到手香提取物11种溶剂残留量

Determination of residual solvents in extract of Coleus amboinicus by headspace-gas chromatography

目的建立顶空-气相色谱法测定中药到手香提取物中苯、丙烯腈、甲基丙烯酸甲酯、甲苯、1,2-二氯乙烷、对二甲苯、间二甲苯、邻二甲苯、氯苯、苯乙烯和二乙烯苯11种溶剂残留的分析方法。方法供试品经顶空进样器85℃平衡45 min,分流比10∶1(V∶V),采用DB-WAX聚乙二醇为固定相的弹性石英毛细管柱(长30 m,内径0.32 mm,膜厚0.5μm),FID氢火焰离子化检测器进行分析。结果11种挥发性有机物分离效果较好,在0.22~23.86μg·mL^(-1)的浓度范围内线性关系良好(r≥0.99);方法定量限为0.0084μg·mL^(-1)≤LOQ≤0.5432μg·mL^(-1);低、中、高水平下各成分的平均回收率为84%~103%之间;相对标准偏差≤10%(n=6),经方法学验证后该方法符合实验要求。3批样品中甲苯、间二甲苯、邻二甲苯及二乙烯基苯有检出,低于定量限,均未超标。结论该方法易于操作,结果可靠,可用于中药到手香提取物中的残留溶剂检测,亦为其他中药提取物中残留溶剂分析提供方法参考,确保用药安全。

Objective To establish a headspace-gas chromatography method for the determination of residues of benzene,acrylonitrile,methyl methacrylate,toluene,1,2-dichloroethane,p-xylene,m-xylene,o-xylene,chlorobenzene,styrene and divinylbenzene in Coleus amboinicus extracts,which is a traditional Chinese medicine(TCM).Methods The samples were balanced by a headspace injector at 85℃for 45 min,and the split ratio was 10:1(V:V).The DB-WAX capillary column(30 m long,0.32 mm wide,and 0.5μm thick),which was fixed using polyethylene glycol,was used to separate samples,while a flame ionization detector(FID)was used for analysis.Results The eleven volatile organic compounds were well-separated.Experimental results showed that the linearity of these volatile organic compounds ranged from 0.22μg·mL^(-1)to 23.86μg·mL^(-1)with correction coefficients above 0.99.The limit of quantification was between 0.0084μg·mL^(-1)and 0.5432μg·mL^(-1).The average recovery of the target compounds ranged from 84%to 103%at three spike levels,with relative standard deviations less than 10.0%(n=6),which met the requirements of trace determination.Toluene,m-xylene,o-xylene and divinylbenzene were detected in three batches of samples,but below the limit of quantitation and the standard.Conclusion This method is simple,reliable,and applicable to the detection of residual solvents in the extract of Coleus amboinicus,which can facilitate the analysis of residual solvents in other TCM extracts and medication safety.