GC-MS/MS法测定医药包装弹性体中的12种亚硝胺

Determination of Twelve Nitrosamines in Medical Packaging Elastomers by GC-MS/MS

建立了气相色谱串联质谱(GC-MS/MS)法同时测定医药包装弹性体密封件中12种亚硝胺,并考察了7种材料在受控提取以及模拟提取条件下12种亚硝胺的提取量。色谱柱采用SH-Stabilwax柱(30 m×0.25 mm×0.25μm),以N-亚硝基二异丙胺(NDiPA)为内标。结果表明,12种亚硝胺在1~60 ng/ml内线性关系良好。在受控提取条件下,12种亚硝胺的加标回收率(n=3)为63.91%~100.90%,RSD为1.0%~4.2%。在pH 2.5、6.5、9.5缓冲液模拟提取介质中,12种亚硝胺的平均回收率(n=3)为73.23%~112.50%,RSD为0.7%~4.6%;在15%乙醇模拟提取介质中,12种亚硝胺的平均回收率(n=3)为93.32%~119.10%,RSD为1.5%~3.2%。本试验建立的方法灵敏度高、专属性好,可用于医药包装弹性体密封件中亚硝胺的测定。

A gas chromatography-tandem mass spectrometry(GC-MS/MS)method was established for the simultaneous determination of twelve nitrosamines in elastomeric closures for pharmaceutical packaging,and the extraction amounts of twelve nitrosamines under controlled extraction and simulated extraction conditions from seven materials were investigated.A SH-Stabilwax column(30 m×0.25 mm×0.25μm)was used,and the N-nitrosodiisopropy lamine(NDiPA)was used as the internal standard.The results showed that twelve nitrosamines were linear in the range of 1–60 ng/ml.Under the controlled extraction condition,the standard recoveries(n=3)of twelve nitrosamines were 63.91%–100.90%,with the RSDs of 1.0%–4.2%.In the simulated extraction media(pH 2.5,6.5,and 9.5 buffer solutions),the average recoveries(n=3)of twelve nitrosamines were 73.23%–112.50%,with the RSDs of 0.7%–4.6%.And in the simulated extraction medium containing 15%ethanol,the average recoveries(n=3)of twelve nitrosamines were 93.32%–119.10%,with the RSDs of 1.5%–3.2%.The established method has high sensitivity and good specificity,which can be used for the determination of nitrosamines in elastomeric closures for pharmaceutical packaging.