GC-MS法测定药用复合包装袋中异氰酸酯

Determination of Isocyanates in Medicinal Composite Packaging Bag by Gas Chromatography-Mass Spectrometry

目的利用气相色谱-质谱(GC-MS)技术建立同时测定药用复合包装袋中8种异氰酸酯含量的方法。方法将药用复合包装袋剪成尺寸(长×宽)不大于5 mm×5 mm的小碎片,采用二氯甲烷超声萃取40 min;萃取液经氮吹浓缩后,采用GC-MS法分析。采用TG-5MS色谱柱,将进样口温度设为200℃,柱温箱初温设为40℃,在程序升温条件下可实现8种异氰酸酯的有效分离。结果8种异氰酸酯在质量浓度为0.02~5.0 mg/L时,线性关系良好,相关系数R^(2)均大于0.997,检出限为0.001~0.006 mg/kg。药用复合包装袋中的异氰酸酯在低、中、高等3个浓度水平下的加标回收率为80.3%~111.7%,相对标准偏差为0.6%~5.1%。结论该方法操作简便、灵敏度高、准确度好,可为药用复合包装袋中异氰酸酯的检测分析提供技术支持。

A method for simultaneous determination of eight isocyanates in medicinal composite packaging bags was established by gas chromatography-mass spectrometry(GC-MS).The composite packaging bag was cut into small pieces no larger than 5 mm×5 mm,and then extracted by dichloromethane for 40 min.The extraction solution was analyzed by GC-MS after concentration by nitrogen blowing.Eight isocyanates could be separated and detected using TG-5MS column with injection temperature of 200℃and initial temperature of column incubator of 40℃.Eight isocyanates had a good linear relationships in the range of 0.02 to 5.0 mg/L with the correlation coefficient greater than 0.997.The detection limit was in the range of 0.001~0.006 mg/kg.The recovery for accuracy at low,medium and high concentration levels was ranged from 80.3%to 111.7%,and the relative standard deviation for repeatability was between 0.6%and 5.1%.This method is simple,sensitive and accurate,which can provide technical support for the detection and analysis of isocyanate in medicinal composite packaging bag.