GC-MS法测定塑料药用滴眼剂瓶中17种邻苯二甲酸酯类塑化剂含量及迁移风险分析

Determination of 17 Phthalic Acid Esters in Plastic Medicinal Eye Drops Bottles by GC-MS and Its Migration Risk Analysis

目的:建立气相色谱-质谱(GC-MS)法测定塑料药用滴眼剂瓶中17种邻苯二甲酸酯(PAEs)含量及其在药品中迁移,并对迁移的塑化剂进行风险评估。方法:样品经正己烷提取,采用HP-5MS(30 m×0.25 mm×0.25μm)毛细管柱程序升温分离,以电子轰击离子源(EI),离子监测(SIM)模式进行检测。结果:17种PAEs在0.05~1μg·mL-1范围内线性关系良好,提取试验和迁移试验平均回收率为72.11%~116.65%,相对平均偏差(RSD)1.23%~6.14%。提取试验20批塑料药用滴眼剂瓶中检出邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二正丁酯(DBP)、邻苯二甲酸二(2-乙基)己酯(DEHP),其中DEHP检出率最高92.31%,其次是DBP为75.00%,迁移试验3批药品中均检出PAEs,分别为DBP、DEHP,对迁移试验检出的DBP、DEHP进行暴露限度评估,结果显示,DBP、DEHP对药品质量的影响可忽略不计,人体健康风险较低。结论:该方法准确、快速,适用于塑料药用滴眼剂瓶中PAEs检测及风险评估。

Objective:Established a gas chromatography-mass spectrometry(GC-MS) method to determine 17 kinds of phthalates(PAEs) in plastic medicinal eye drop bottles and their migration in medicines. And analyzed the migration of plasticizers by risk assessment. Methods:The samples were extracted with n-hexane and separated by temperature-programmed capillary column using HP-5 MS(30 m×0.25 mm×0.25 μm), and detected by electron bombardment ion source(EI) and ion monitoring(SIM) mode. Results: The 17 PAEs had a good linear relationship in the range of 0.05-1 μg·mL-1. The average recovery rate of extraction test and migration test was 72.11%-116.65%. The relative mean deviation(RSD) was 1.23%-6.14%.Diisobutyl phthalate(DIBP), Dibutyl phthalate(DBP) and bis(2-ethylhexyl) phthalate(DEHP) were detected in 20 batches of plastic medicinal eye drop bottles in the extraction test.The highest detection rate of DEHP was 92.31%, followed by DBP was 75.00%.And PAEs were detected in all three batches of drugs in the migration test, which were DBP and DEHP respectively. The exposure limits of DBP and DEHP detected in the migration test were evaluated. The results showed that the impact of DBP and DEHP on drug quality is negligible.And the risk to human health was low.Conclusion:This method is accurate and rapid.And it is suitable for the detection and risk assessment of PAEs in plastic medicinal eye drop bottles.