提出了电感耦合等离子体质谱法(ICP-MS)测定丙氨酰谷氨酰胺注射液中铝含量的方法。移取供试品7.5 mL共6份,分别置于6个15 mL塑料离心管中,各加入一定量的铝标准溶液,再用5%(体积分数)硝酸溶液稀释至刻度,摇匀,经0.22 μm水膜过滤,得到供试品加标溶液系列,标准加入法定量。ICP-MS分析中选择雾化气稀释高基体样品引入-氦气碰撞(HMI-He)模式。结果显示:某供试品加标溶液中铝的质量浓度在30.00 μg·L^-1内与其对应的响应值呈线性关系,检出限(3s)为0.88 μg·L^-1;对供试品加标溶液进行精密度试验,铝测定值的相对标准偏差(n=6)均小于2.0%;对同一供试品进行3个浓度水平的加标回收试验,回收率为101%~106%。方法用于12批丙氨酰谷氨酰胺注射液的分析,铝的检出量为20.00~31.22 μg·L^-1。

A method for the determination of aluminum in alanyl glutamine injection by inductively coupled plasma mass spectrometry (ICP-MS) was proposed. 6 test samples (7.5 mL) were placed in 6 plastic centrifuge tubes of 15 mL, and a certain amount of aluminum standard solutions was added. Then the test spiked solution series were diluted by 5% (φ) nitric acid solution, and filtered by 0.22 μm water membrane. Standard addition method was used for quantitative analysis. Atomized gas to dilute high matrix sample introduction helium collision (HMI-He) mode was used for ICP-MS analysis. As shown by the results, linear relationship between value of mass concentration of aluminum in a test spiked solutions and its response value was kept within 30.00 μg·L^-1, with detection limit (3s) of 0.88 μg·L^-1. Test spiked solutions were determined for precision, and RSDs (n=6) of the determined values were less than 2.0%. Recovery test was made on the same test sample at 3 concentration levels by standard addition method, giving results in the range of 101%-106%. This method has been applied to the analysis of 12 batches of alanyl glutamine injections, and detection amounts of aluminum were in the range of 20.00-31.22 μg·L^-1.