布洛芬注射液包材相容性研究中铅、镉、砷、锑的测定

Determination of lead,cadmium,arsenic and antimony in ibuprofen injection of drug compatibility study

建立中性硼硅玻璃包材加速试验后布洛芬注射液中铅、镉、砷、锑含量的检测方法。采用微波消解仪以硝酸分解样品,用石墨炉原子吸收光谱仪测定铅、镉含量,测定波长铅为283.3 nm,镉为228.8 nm,铅、镉分别在5.0~50.0,0.5~5.0μg/L范围内有良好的线性,相关系数分别为0.999 7,0.996 2,检出限分别为0.26,0.01μg/L,测定结果的相对标准偏差分别为1.06%,2.40%(n=6),加标回收率分别为100.2%~101.9%,97.1%~105.1%。用原子荧光光谱仪测定砷、锑含量,测定波长砷为193.7 nm,锑为217.6 nm,砷、锑在1~10μg/L范围内均有良好的线性,相关系数分别为0.999 9,0.999 5,检出限分别为0.03,0.01μg/L,测定结果的相对标准偏差分别为1.04%,2.65%(n=6),加标回收率分别为94.2%~96.5%,92.6%~96.5%。该测定方法快速,灵敏度高,适用于内包装材料加速试验后药品中重金属元素含量变化的研究。

A method was established for the determination of trace lead,cadmium,arsenic and antimony in ibuprofen injection after the accelerated testing of neutral borosilicate glass packaging materials.Samples were digested by nitric acid in the microwave digestion apparatus.Lead and cadmium were determined by graphite furnace atomic absorption spectrometer.The detection wavelength was 283.3 nm for lead and 228.8 nm for cadmium.Their linear ange were 5.0-50.0,0.5-5.0μg/L,teh correlation coefficients were 0.999 7,0.996 2,and detection limits were 0.26,0.01μg/L,repectively.The relative standard deviations of lead,cadmium detection resuls were 1.06%,2.40%(n=6),and the recoveries were 100.2%-101.9%,97.1%-105.1%,respectively.Arsenic and antimony were determined by hydride generation atomic fluorescence spectrometry.The detection wavelength was 193.7 nm for arsenic,and 217.6 nm for antimony.Both arsenic and antimony showed good linear relationship in the range of 1-10μg/L,correlation coefficients were 0.999 9,0.999 5,repectively.The detection limits of arsenic and antimony were 0.03,0.01μg/L,the relative standard deviations of detection results were 1.04%,2.65%(n=6),and the recoveries were 94.2%-96.5%,92.6%-96.5%,respectively.The method is fast and sensitive,which can be used for the determination of trace heavy metal elements in ibuprofen injection after the accelerated testing.