采用微波消解-电感耦合等离子体质谱(ICP-MS)测定法考察蚓激酶中有害元素的残留量

目的：建立测定蚓激酶中铬（Cr）、锰（Mn）、铁（Fe）、钴（Co）、镍（Ni）、铜（Cu）、砷（As）、银（Ag）、镉（Cd）、锑（Sb）、钡（Ba）、汞（Hg）、铊（Tl）、铅（Pb）14个有害元素含量的方法。方法：采用微波消解-电感耦合等离子体质谱法，射频功率为1 530 W，冷却温度为4℃，碰撞气为氦气，载气为氩气，载气流量为1.08 L&#183;min^-1，积分时间为0.3 s，等离子气流量为15 L&#183;min^-1，四极杆真空度为3.04&#215;10^-4 Pa，采样锥孔径为1.0 mm，截取锥孔径为0.4 mm，数据采集重复次数为3次。结果：Mn、Ni与Cu元素检测线性范围为0~500 ng&#183;mL^-1，Fe元素检测线性范围为0~10 000 ng&#183;mL^-1，Hg元素检测线性范围为0~10 ng&#183;mL^-1，其余各元素检测线性范围均为0~100 ng&#183;mL^-1，r均≥ 0.999 0；检测下限为0.004~0.7 ng&#183;mL^-1；精密度的RSD<2%，重复性的rsd<8%；各元素平均加样回收率为95.4%~109.8%（rsd<4%，n=9）。结论：该方法线性回归良好，灵敏度高，准确性好，适用于蚓激酶原料药中有害元素的检测分析。

Objective: To establish a determination method of Cr, Mn, Fe, Co, Ni, Cu, As, Ag, Cd, Sb, Ba, Hg, Tl and Pb in lumbrokinase. Methods: Microwave digestion-inductively coupled plasma mass spectrometry (MD-ICPMS) was adopted. RF power was 1 530 W, cooling temperature was 4℃,collision gas was He gas,the flow rate of the carrier gas (argon gas) was 1.08 L&#183;min^-1, integration time was 0.3 s, plasma gas flow rate was 15 L&#183;min^-1,the vacuum degree of quadrupole was 3.04&#215;10^-4 Pa,sampling cone aperture was 1.0 mm,interception cone aperture was 0.4 mm,and the data collection was repeated 3 times. Results: The linear ranges of Mn,Ni and Cu were 0-500 ng&#183;mL^-1 (r ≥ 0.999 0), the linear range of Fe was 0-10 000 ng&#183;mL^-1,the linear range of Hg was 0-10 ng&#183;mL^-1 and the linear ranges of other elements were 0-100 ng&#183;mL^-1 (r ≥ 0.999 0). RSDs of precision tests were lower than 2.0% and RSDs of reproducibility tests were lower than 8.0%. Average recoveries were 95.4%-109.8% (RSD<4%, n=9). Conclusion: With good linear relationship, sensitivity and accuracy, the method is suitable for detection of harmful elements in lumbrokinase.

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