微波消解-电感耦合等离子体质谱法测定祖师麻中重金属元素含量
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摘要
采用微波消解技术建立电感耦合等离子体质谱法测定中药祖师麻中重金属Pb、Cd、Cr、As、Hg、Cu、Zn含量的方法。将样品进行微波消解,完善前处理条件,优化ICP-MS的工作参数。选取72Ge、115In、209Bi、103Rh、45Sc、6Li、159Tb、89Y作为内标元素,有效克服基体效应及仪器波动影响。采用Qcell碰撞池技术、KED模式降低了多原子干扰。测定元素标准曲线相关系数R2均在0.995以上,各元素检出限在0.003～0.193 g/L之间。用国家标准物质评价了方法准确性。研究表明,该方法线性范围宽、准确性高、精密度好,适用于快速测定不同产地的祖师麻中重金属含量,也可用于中药材的质量控制。
With microwave digestion technique, inductively coupled plasma mass spectrometry(ICP-MS) is applied to determine heavy metals such as Pb, Cd, Cr, As, Hg, Cu and Zn in Zushima(Girald daphne bark). The samples are put into microwave for digestion pretreatment to optimize parameters of ICP-MS. Elements such as 72 Ge, 115 In, 209 Bi, 103 Rh, 45 Sc, 6 Li, 159 Tb and 89 Y are selected as internal standard elements to reduce the influence of matrix and instrument fluctuations. Qcell collision cell technology and KED mode are employed to reduce polyatomic interference. The correlation coefficient R2 of the elemental standard curve is above 0.995, and the detection limit of each element is between 0.003 ～ 0.193 g/L. The accuracy of the method is evaluated by national standard materials and the results indicate that the method is with wide linear range. It is accurate and suitable for rapid determination of heavy metal content in the Zushima of different raw materials, and quality control of Chinese medicinal materials.
With microwave digestion technique, inductively coupled plasma mass spectrometry(ICP-MS) is applied to determine heavy metals such as Pb, Cd, Cr, As, Hg, Cu and Zn in Zushima(Girald daphne bark). The samples are put into microwave for digestion pretreatment to optimize parameters of ICP-MS. Elements such as 72 Ge, 115 In, 209 Bi, 103 Rh, 45 Sc, 6 Li, 159 Tb and 89 Y are selected as internal standard elements to reduce the influence of matrix and instrument fluctuations. Qcell collision cell technology and KED mode are employed to reduce polyatomic interference. The correlation coefficient R2 of the elemental standard curve is above 0.995, and the detection limit of each element is between 0.003 ～ 0.193 g/L. The accuracy of the method is evaluated by national standard materials and the results indicate that the method is with wide linear range. It is accurate and suitable for rapid determination of heavy metal content in the Zushima of different raw materials, and quality control of Chinese medicinal materials.
引文
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[3] 李宇伟,王新民,连瑞丽,等.微波消解-电感耦合等离子体质谱法测定怀牛膝中重金属元素含量[J].安徽农业科学,2008,36(33):14582-14584.
[4] 何军民,杨鸽华,闫志健,等.祖师麻总香豆素的提取工艺研究[J].海峡药学,2011,23(12):86-88.
[5] 任燕冬,杨武亮,宋宏杉,等.祖师麻质量控制研究[J].中成药,2009(6):950-953.
[6] 赵小学,张霖琳,张建平,等.ICP-MS在环境分析中的质谱干扰及其消除[J].中国环境监测,2014,30(3):101-103.
[7] 周勇义,谷学新,范国强,等.微波消解技术及其在分析化学中的应用[J].冶金分析,2004,24(2):30-32.
[8] 中华人民共和国商务部.药用植物及制剂进出口绿色行业标准[M].北京:中国标准出版社,2005.
[9] 中华人民共和国药典委员会.中国药典[M].北京:中国医药科技出版社,2015.