摘要
目的:测定门冬氨酸钾镁注射液中钾、镁与杂质钠含量。方法:建立电子稀释技术电感耦合等离子体质谱法(EDR-ICP-MS)同时测定门冬氨酸钾镁注射液中钾、镁和钠的含量。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。采用新建立的ICP-MS法与法定标准的滴定法和重量法分别对来源于6个厂家的29批次样品进行测定和统计分析。结果:钾、镁和钠的线性范围分别为44~70μg·ml^(-1)(r=1.0000)、16~26μg·ml^(-1)(r=1.0000)和0.5~5.0μg·ml^(-1)(r=1.0000);回收率分别为101.0%,101.4%,101.0%,RSD分别为1.3%,1.2%,0.7%(n=9)。29批次样品的测定结果经统计分析,两种测定方法测定的镁含量差异无统计学意义(P>0.05),而钾含量差异有统计学意义(P<0.05),且ICP-MS法专属性更强。钠离子含量为0.04~0.81 mg·ml^(-1),不同企业差异间含量差异较大。结论:所建立的ICP-MS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 content determination method for K^(+),Mg^(2+) and Na^(+) in potassium and magnesium aspartate injection by EDR-ICP-MS.Methods:An EDR-ICP-MS method was established for the simultaneous determination of K^(+),Mg^(2+) and Na^(+) in potassium and magnesium aspartate injection.The specificity,precision,recovery and linearity of the established method were verified.Totally 29 batches of samples from 6 manufacturers were analyzed respectively by the ICP-MS method,titration method and gravimetric method.Results:The linear ranges of K^(+),Mg^(2+) and Na^(+) were 44-70μg·ml^(-1)(r=1.0000),16-26μg·ml^(-1)(r=1.0000)and 0.5-5.0μg·ml^(-1)(r=1.0000),respectively;the recoveries were 101.0%,101.4%,101.0%with the RSDs of 1.3%,1.2%and 0.7%(n=9),respectively.The results of 29 batches of samples were statistically analyzed by paired t-test.The statistical results showed that there was no significant difference in the determination of Mg^(2+) (P>0.05),while there was a significant difference in the determination of K^(+)(P<0.05).Conclusion:The established EDR-ICP-MS method is simple,specific,accurate,reliable and rapid,and suitable for the analysis of batch samples,and can be used for the quality evaluation and control of potassium and magnesium aspartate injection.
作者
高丽琼
彭彦
Gao Liqiong;Peng Yan(Hangzhou Institute for Food and Drug Control,Hangzhou 310022,China)
出处
《中国药师》
CAS
2022年第10期1861-1864,共4页
China Pharmacist
关键词
电感耦合等离子体质谱
门冬氨酸钾镁注射液
钾
镁
钠
含量测定
Inductively coupled plasma mass spectrometry
Potassium and magnesium aspartate injection
K^(+)
Mg^(2+)
Na^(+)
Content determination
