二次微波消解-电感耦合等离子体质谱联用技术同时测定蒙脱石原料及其制剂中的三氧化二铝、二氧化硅及氧化镁  

Simultaneous determination of aluminum trioxide,silicon dioxide,and magnesium oxide in montmorillonite raw materials and their formulations using secondary microwave digestion inductively coupled plasma mass spectrometry technology

作　　者：陈真 谢静[2] 石峰 咸瑞卿 巩丽萍 杭宝建 由鹏飞 陈晓 张冬梅 CHEN Zhen;XIE Jing;SHI Feng;XIAN Rui-qing;GONG Li-ping;HANG Bao-jian;YOU Peng-fei;CHEN Xiao;ZHANG Dong-mei(Shandong Institute for Food and Drug Control,Jinan 250101,China;Qilu Hospital of Shandong University,Jinan 250063,China)

机构地区：[1]山东省食品药品检验研究院,济南250101 [2]山东大学齐鲁医院,济南250063

出　　处：《药物分析杂志》2024年第4期577-584,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：山东省重点研发计划(2022TZXD004);泰山产业领军人才工程专项经费资助。

摘　　要：目的:建立一种同时测定蒙脱石及其制剂中三氧化二铝、二氧化硅及氧化镁3个成分的含量测定方法。方法:采用稀硝酸-氢氟酸-饱和硼酸溶液二次微波消解与电感耦合等离子体质谱(ICP-MS)联用技术,优化建立以铑(103Rh)为内标可同时测定蒙脱石中铝(27Al)、硅(28Si)及镁(24Mg)3个元素的分析方法,并分别与《中华人民共和国药典》二部中EDTA容量法测定三氧化二铝、马弗炉炽灼燃烧法测定二氧化硅,美国药典偏硼酸锂熔融样品后原子吸收分光光度法测定氧化镁的测定方法进行了比较分析。结果:建立的蒙脱石测定三氧化二铝、二氧化硅及氧化镁含量分析方法,铝(Al)和硅(Si)的线性均在25~300 ng·mL^(-1),镁(Mg)的线性在20~240 ng·mL^(-1),r≥0.999;Al、Si、Mg的检测限依次为0.49、1.30、0.71 ng·mL^(-1),各剂型的平均回收率依次在99.7%~100.6%、99.9%~101.2%、99.8%~101.2%,重复性RSD(n=6)依次为0.3%~1.3%、0.4%~1.2%、0.4%~1.0%。采用新建方法和原标准方法分别测得蒙脱石中三氧化二铝的含量依次为2.3%~2.4%、2.0%~2.2%,二氧化硅的含量依次为58.7%~61.5%、55.3%~59.4%,氧化镁的含量依次为15.9%~20.6%、14.6%~19.4%,测定结果基本一致。结论:本文采用的二次微波消解与ICP-MS联用方法简单快捷,灵敏度高,准确性好,可用于蒙脱石原料及制剂的三氧化二铝、二氧化硅及氧化镁含量测定。Objective:To establish a method for simultaneous determination of aluminum trioxide,silicon dioxide and magnesium oxide in montmorillonite and its preparations.Methods:The method was optimized and estab⁃lished for simultaneous determination of aluminum(27Al),silicon(28 Si),and magnesium(24Mg)in montmoril⁃lonite using rhadium(103Rh)as the internal standard,a dilute nitric acid hydrofluoric acid saturated boric acid solution with secondary microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS).The method was compared and analyzed with the EDTA volumetric method for the determination of aluminum trioxide,the muffle ignition combustion method for the determination of silicon dioxide and the AAS method for the determi⁃nation of magnesium oxide after melting samples of lithium metaborate in the USP.Results:The linear of alumi⁃num(Al)and silicon(Si)were in the range of 25-300 ng·mL^(-1).The linear of magnesium(Mg)was in the range of 20-240 ng·mL^(-1),r≥0.999.The detection limits of Al,Si,and Mg were 0.49,1.30,0.71 ng·mL^(-1).The average recoveries were 99.7%-100.6%,99.9%-101.2%,99.8%-101.2%,and the average repeatability RSDs(n=6)were 0.3%-1.3%,0.4%-1.2%,and 0.4%-1.0%.The contents of aluminum trioxide,silicon dioxide and magnesium oxide in montmorillonite,montmorillonite powder,and mont⁃morillonite dispersion tablets were determined using the newly established method and the original standard meth⁃od,and the measurement results were basically consistent.Eight common peaks were identified from fingerprints of 10 batches of samples.The RSD values of relative retention time of 8 common peaks of chromotograms of sam⁃ples were all below 0.5%and the similarities were above 0.9.The contents of aluminum trioxide in montmorillon⁃ite were determined using the newly established method and the original standard method,which were 2.3%to 2.4%,2.0%to 2.2%,58.7%to 61.5%,55.3%to 59.4%,and 15.9%to 20.6%,14.6%to 19.4%,respectively.The results of the measurements were basically consistent for the d

关 键 词：蒙脱石 蒙脱石散 蒙脱石分散片 三氧化二铝 二氧化硅 氧化镁 微波消解 电感耦合等离子体质谱法 

分 类 号：R917[医药卫生—药物分析学]