ICP-MS法测定复方苦参注射液中铜、砷、镉、汞、铅元素的残留量

目的：建立复方苦参注射液中铜、砷、镉、汞、铅5种元素残留量的测定方法。方法：样品经消解后采用电感耦合等离子体质谱法（ICP-MS法）测定，射频功率为1 550 W，载气（高纯氩气）流速为1.05L·min^-1，等离子气体流速为15.0 L·min^-1，蠕动泵转速0.2 r·s^-1，采样深度10 mm，重复次数为3次。通过在线加入内标锗、铟、铋元素的方法来校正基体效应和干扰。结果：各元素在各自的检测质量浓度范围内线性关系良好（r>0.999 8），进样精密度RSD在0.8%~1.5%，重复性RSD在1.8%~6.4%，5种元素高、中、低3种浓度的加样回收率在78.9%~106.4%，样品在消解后48 h内各元素稳定性良好，铜、砷、镉、汞、铅检测下限分别为24.04、35.92、4.84、5.43、16.18 pg·mL^-1，定量下限分别为80.13、119.72、16.13、18.10、53.94 pg·mL^-1。10批样品中铜含量范围为0~17.16 ng·mL^-1，砷含量范围为6.07~11.04 ng·mL^-1，镉含量范围为0.04~0.71 ng·mL^-1，汞含量范围为0~1.14 ng·mL^-1，铅含量范围为2.43~12.43 ng·mL^-1，5种元素含量均在合格范围内。结论：本方法可用于复方苦参注射液中铜、砷、镉、汞、铅5种元素的含量测定。

Objective:To develop a method for the determination of residues of copper(Cu), arsenic(As), cadmium(Cd), mercury(Hg) and lead(Pb) in compound Kushen injection.Methods:Samples were digested by microwave and measured with ICP-MS.The RF power was 1 550 W and the current velocity was 1.05 L·min^-1.Plasma gas velocity was 15.0 L·min^-1.Peristaltic pump speed was 0.2 r·s^-1 and the sampling depth was 10 mm.The signal was measured for 3 times.The internal standard solution of Ge, In and Bi were used for matrix effect correction.Results:The linearities for the elements were good with the correlation coefficients(r) being all above 0.999 8.The RSDs of the injection precision test were in the range of 0.8%-1.5% and the RSDs of the repeatability test were in the range of 1.8%-6.4%.The average recoveries of the 5 elements at three levels(high, medium and low concentration) were in the range of 78.9%-106.4%, and the digested solution was stable in 48 h.The detection limits of Cu, As, Cd, Hg and Pb were 24.04, 35.92, 4.84, 5.43 and 16.18 pg·mL^-1 and the quantitation limits were 80.13, 119.72, 16.13, 18.10, 53.94 pg·mL^-1, respectively.In 10 batches of samples, the contents of Cu, As, Cd, Hg and Pb ranged from 0 to 17.16 ng·mL^-1, 6.07 to 11.04 ng·mL^-1, 0.04 to 0.71 ng·mL^-1, 0 to 1.14 ng·mL^-1 and 2.43 to 12.43 ng·mL^-1, respectively, which were all in the acceptable ranges.Conclusion:The method can be used for the content determination of Cu, As, Cd, Hg and Pb in compound Kushen injection.