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. 5 μg/L, and limits of quantitation were 0. 3-28. 3 μg/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.%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800 W, 消解程序为升温至120 ℃保持3min,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1150 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. 0mg/L,硒、铅为0. 4~4. 0 mg/L(r均≥0. 9995);检测限为0. 1~8. 5 μg/L;定量限为0. 3~28. 3 μg/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.
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