ICP-OES法同时测定门冬氨酸钾镁注射液中钾离子和镁离子的含量

Simultaneous determination of principal ions K^+ and Mg^(2+) in the potassium aspartate and magnesium aspartate injection by ICP-OES

目的:建立电感耦合等离子体原子发射光谱(ICP-OES)法同时测定门冬氨酸钾镁注射液中钾离子和镁离子的含量。方法:根据专属性高、干扰小的原则,分别选择766.490 nm和279.553 nm作为钾和镁的分析谱线,建立ICP-OES法同时测定门冬氨酸钾镁注射液中钾离子和镁离子的含量。对所建立的方法进行专属性、精密度、回收率和线性等方法学验证。采用新建的ICP-OES法与传统的滴定法和重量法分别对来源于2个厂家的5批样品同时进行测定和统计学分析。结果:钾离子和镁离子的线性范围分别为5~25μg·mL^(-1)(r^2=0.999 1)、1~9μg·mL^(-1)(r^2=0.999 5);钾离子和镁离子高、中、低3种浓度的回收率分别在98.3%~100.0%和98.5%~101.5%,RSD分别为0.6%(n=9)和0.9%(n=9)。5批样品的测定结果经t检验统计分析,统计结果 p>0.05,表明ICP-OES法与传统测定方法无显著性差异,可以替代传统方法进行钾离子和镁离子的含量测定。结论:所建立的ICP-OES法操作简单,专属性强,准确可靠、分析快速,具有多元素同时测定的特点,适合于批量样品的分析,可用于门冬氨酸钾镁注射液的质量评价和控制。

Objective： To establish a method for simultaneous determination of the content of principal ions K＋ and Mg2＋ in the potassium aspartate and magnesium aspartate injection by inductively coupled plasma-atomic emission spectrometry （ICP-OES）.Methods： An ICP-OES method was established to determine the content of K＋ and Mg2＋ in the potassium aspartate and magnesium aspartate injection.Based on the principle of specificity and interference,766.490 nm and 279.553 nm were selected as the analytical spectral lines for K＋ and Mg2＋,respectively.And the established method was proved by methodology validation such as specificity,precision,recovery and linearity.Finally,5 batches of samples which derived from two factories were determined by the established ICP-OES method and the conventional methods such as titration method and weight method.The results were statistically analyzed.Results： The calibration curve was linear over the range of 5-25 μg·mL-1（r2=0.999 1）for K＋、1-9 μg·mL-1（r2=0.999 5） for Mg2＋.The recoveries of K＋ were between 98.3% and 100.0% at high-medium and low concentrations,while those of Mg2＋ were between 98.5% and 101.5%.The relative standard derivations of K＋ and Mg2＋ were 0.6% （n=9） and 0.9% （n=9）,respectively.The results of the five batches of samples showed p〉0.05 which were analyzed by t test.The data indicated that ICP-OES method and the traditional method had no significant differences,and the established ICP-OES method could be used to replace the traditional method.Conclusion： The established ICP-OES method is proved by methodology validation.It is convenient,specific,accurate and rapid.It has the characteristics of simultaneous multi-element determination and it is suitable for the analysis of batches of samples.And it is applicable for the quality control of potassium aspartate and magnesium aspartate injection.