GC/MS测定明胶空心胶囊中17种塑化剂

Determination of 17 kinds of plasticizer in Vacant gelatin capsules by chromatography-mass spectrometry

目的:建立气相色谱/质谱联用检测明胶空心胶囊中17种塑化剂,包括邻苯二甲酸二异壬酯(DINP)的方法。方法:粉碎均匀样品用乙腈提取,超声提取30min后取上层清液用气相色谱/质谱联用仪测定。结果:17种塑化剂的线性关系较好,方法检出测限范围在0.01~0.24mg/kg,在高、中、低3个水平下进行明胶空心胶囊样品加标实验,平均回收率为86.68%~104.21%,相对标准偏差2.69%~5.11%(n=6)。结论:明胶空心胶囊用乙腈提取比用正己烷等溶剂提取效果好,同时方法的检出限低,且该方法简便、快捷,溶剂用量小、重现性好。

Objective：The method was established lbr the determination of 17 kinds of plasticizer （PAEs,incluiding DINP）in Vacant gelatin capsules by gas chromatography/mass spectrometry.Methods：The PAEs in the Cnshing uniform sample were extraction by acetonitrile,Uhrasonic extraction after 30min take supernatant liquid gas and directly detected with gas chromatography spectrometry （GC-MS）.Results：The PAEs content was analyzed and it was in good linear relationship.The detection limits of 17 PAEs were from 0.01mg/kg to 0.24mg/kg.The recovery range was between 86.68% and 104.21% in low,middle and higher level standard addition experiments.The relative standard deviations were between 2.69% and 5.11%（ n=6 ）.Conclusion：The acetonitrile solvent precedes n-hexane using were extracted 17 kinds of plasticizer in Vacant gelatin capsules and significantly lower the detection limits.The method is simple,accurate,and has good reproducibility;meanwhile the solvent consmnption is small in this method.