GC-MS法测定一次性使用静脉营养输液器中增塑剂DEHP的溶出量

目的:建立测定一次性使用静脉营养输液器中增塑剂邻苯二甲酸二(2-乙基己基)酯(DEHP)溶出量的方法。方法:采用气相色谱-质谱联用(GC-MS)法,以邻苯二甲酸二丁酯为内标,使用一次性使用静脉营养输液器制备营养液,测定室温放置和模拟临床输液24 h后营养液中DEHP的溶出量。采用Rtx-5 MS色谱柱;进样口温度:300℃;载气:氦气;程序升温模式:起始温度200℃,15℃/min升温至280℃,维持5 min;EI离子源,离子源温度:250℃,接口温度:280℃;采集模式:选择离子监测模式(SIM):质荷比(m/z)149。结果:DEHP检测质量浓度的线性范围为0.2³0μg/m(lr=0.999 8),检测限为0.01μg/ml,定量限为0.04μg/ml,平均回收率为102.4%,RSD为4.23%(n=3),精密度试验RSD为2.7%(n=5)。室温放置24 h营养液中DEHP溶出量为0.54730μg/m(lr=0.999 8),检测限为0.01μg/ml,定量限为0.04μg/ml,平均回收率为102.4%,RSD为4.23%(n=3),精密度试验RSD为2.7%(n=5)。室温放置24 h营养液中DEHP溶出量为0.547¹7.400 mg,模拟临床输液24 h后营养液中DEHP溶出量为8.77917.400 mg,模拟临床输液24 h后营养液中DEHP溶出量为8.779¹0.620 mg,均小于成人的耐受摄入量(30 mg)。结论:本法简单、快速、准确,可用于一次性使用静脉营养输液器中DEHP溶出量的测定。

Determination of DEHP Released from Disposable Venous Nutrition Transfusion Instruments by GC-MS

OBJECTIVE： To establish the method for the determination of the dissolution of di （2-ethyl hexyl） phthalate （DEHP） from disposable venous nutrition transfusion instruments. METHODS： GC-MS analysis was performed. Using dibutyl phthalate as internal standard, the determination was performed on Rtx-5 MS column with injector temperature of 300 ℃ using helium as carrier gas by temperature programming： initial temperature 200 ℃, increasing to 280 ℃ at rate of 15 ℃/min maintained for 5 min. EI ion source was adopted with temperature of 250 ℃ in acquisition mode; the injector temperature was set at 280 ℃. The ion moni- toring mode was SIM, and the selected ion was m/z 149. RESULTS： The linear range of DEHP was 0.2-30 μg/ml （r=0.999 8） with an average recovery of 102.4% （RSD=4.23%, n=3）. The detection limit was 0.01 μg/ml, and the limit of quantification was 0.04 μg/ml. RSD of precision test was 2.7% （n=5）. The dissolution of DEHP were 0.54%17.400 mg at room temperature for 24 hours. The dissolution of DEHP were 8.779-10.620 mg after 24 h simulated use in the clinic, which were not more than the limit of tolerance intake （30 mg）. CONCLUSIONS： The method is simple, rapid and accurate, and can be used for the determination of DEHP released from disposable venous nutrition transfusion instruments.