电感耦合等离子体发射光谱法测定十全大补丸中12种微量元素含量的方法研究  

Content Determination of 12 Trace Elements in Shiquan Dabu Pills by ICP-OES

作　　者：康璧 朱琼 吴芸 KANG Bi;ZHU Qiong;WU Yun(Taizhou Institute for Food and Drug Control,Jiangsu Taizhou 225300,China)

机构地区：[1]泰州市食品药品检验所,江苏泰州225300

出　　处：《中国药房》2018年第5期637-639,共3页China Pharmacy

摘　　要：目的:建立测定十全大补丸中12种微量元素(铜、锰、镁、镉、锌、铁、钡、硒、铅、砷、铬、镍)含量的方法,为进一步完善其质量控制提供参考。方法:采用电感耦合等离子体原子发射光谱法(ICP-OES)。采用微波消解法进行样品前处理,消解功率为800W,消解程序为升温至120℃保持3 min,然后升温至160℃保持5 min,最后升温至180℃保持20 min。等离子体功率为1 150 W,泵速为50 r/min,雾化气流速为0.5 L/min,等离子气体流速为12.0 L/min,检测波长为182.205~455.403 nm。结果:以国家标准物质进样测定发现12种元素测定结果均在标准值范围内。铜、锰、镁、镉、锌、铁、钡、砷、铬、镍检测的线性范围均为0.2~2.0 mg/L,硒、铅为0.4~4.0 mg/L(r均≥0.999 5);检测限为0.1~8.5μg/L;定量限为0.3~28.3μg/L;精密度试验的RSD均<1.00%(n=6);平均回收率为88.5%~99.0%(RSD为1.7%~4.9%,n=6)。结论:该方法快速、简便、灵敏度高,可用于十全大补丸中12种微量元素的含量测定。OBJECTIVE:To establish the method for content determination of 12 trace elements(Cu,Mn,Mg,Cd,Zn,Fe,Ba,Se,Pb,As,Cr,Ni)in Shiquan dabu pills,and to provide reference for further improvement of its quality control.METHODS:ICP-OES was adopted to detect.Microwave digestion was used for sample pretreatment with digestion power of 800 W;digestion process included heating to 120℃keeping for 3 min,heating to 160℃keeping for 5 min,and finally heating to 180℃keeping for 20 min.PF power was 1 150 W,and pump speed was 50 r/min;the flow rate of atomizing gas was 0.5 L/min,and that of plasma gas was 12.0 L/min,detection wavelength of 182.205-455.403 nm.RESULTS:Results of 12 elements determination were all within standard range according to national standard substance sampling determination.The liner ranges of Cu,Mn,Mg,Cd,Zn,Fe,Ba,As,Cr and Ni were 0.2-2.0 mg/L,those of Se and Pb were 0.4-4.0 mg/L(r≥0.999 5).The detection limits ranged 0.1-8.5μg/L,and limits of quantitation were 0.3-28.3μg/L.RSDs of precision tests were all lower than 1.00%(n=6).The average recovery rates were 88.5%-99.0%(RSD were 1.7%-4.9%,n=6).CONCLUSIONS:The method is rapid,simple and sensitive,and it can be used for content determination of 12 trace elements in Shiquan dabu pills.

关 键 词：十全大补丸 微波消解 电感耦合等离子体发射光谱法 微量元素 含量测定 

分 类 号：R917[医药卫生—药物分析学]