HPLC-ICP-MS联用测定小儿咳喘灵颗粒中Cr(Ⅵ)和Cr(Ⅲ)

Determination of Chromium(Ⅵ)and Chromium(Ⅲ)in Xiaoer Kechuanling Granules by Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

目的:采用高效液相色谱-电感耦合等离子体质谱联用法(HPLC-ICP-MS)测定小儿咳喘灵颗粒中六价铬和三价铬含量。方法:参照EPA Method 3060A方法碱提六价铬,微波消解提取三价铬,使用Hamilton PRP-X100(250 mm×4.1 mm,10μm)色谱柱,流动相为0.075 mol·L^-1硝酸铵溶液,ICP-MS分析同位素52 Cr、He模式。结果:六价铬和三价铬在5~100μg·L-1线性关系良好(r>0.999),Cr(Ⅵ)加样回收率为82.1%~90.4%;Cr(Ⅲ)加样回收率为94.1%~95.2%。8批样品均检出Cr(Ⅵ),检出值为0.027~0.082μg·g-1,平均值为0.051μg·g^-1,Cr(Ⅲ)检出值为5.775~18.743μg·g^-1,平均值为10.366μg·g^-1。结论:实验所建方法准确可靠,为更客观、合理地评价中成药中铬的安全性提供参考。

Objective:To determine the content of chromium(Ⅵ)and chromium(Ⅲ)in Xiaoer Kechuanling Granules by HPLC-ICP-MS.Methods:With reference to EPA Method 3060A,chromium(Ⅵ)was extracted by alkali extraction,and chromium(Ⅲ)was extracted by microwave digestion.Hamilton prp-X100(250 mm×4.1 mm,10μm)chromatographic column was used.The mobile phase was 0.075 mol/L ammonium nitrate solution.Isotope 52 Cr was analyzed by ICP-MS in He mode.Results:The standard curves of chromium(Ⅵ)and chromium(Ⅲ)had good linear relationship in 5-100μg·L-1 concentration range(r>0.999).The average recoveries of chromium(Ⅵ)were 82.1%-90.4%and chromium(Ⅲ)were 94.1%-95.2%.Estimated value of chromium(Ⅵ)ranged from 0.027 to 0.082μg·g^-1 and mean value was 0.051μg·g^-1.chromium(Ⅲ)tested ranged from 5.775 to 18.743μg·g-1,then average value was 10.366μg·g^-1.Conclusion:The method is accurate and reliable,providing reference for more objective and reasonable evaluation of the safety of chromium in Chinese patent medicine.