高效液相色谱-电感耦合等离子体质谱(ICP-MS)法测定中药材中无机汞、甲基汞、乙基汞

目的 建立中药材中无机汞、甲基汞、乙基汞的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)测定方法,考察106批次根及根茎类中药材中3种汞形态化合物的含量,积累基础数据,为中药饮片的质量安全性监管提供技术支撑。方法 选用人工胃液作为提取液,经水浴加热提取后,以甲醇-乙酸铵为流动相,采用C18反相色谱柱对样品溶液进行分离,最后经ICP-MS测定3种汞形态化合物的含量。结果 3种汞形态化合物在0.5～5ng/mL范围内均获得良好的线性关系,相关系数均大于0.999。通过加标回收的方法进行准确性评价,回收率为75.5%～118.0%,RSD为2.4%～9.7%。测定的106批次中药材中,均未检出甲基汞、乙基汞。无机汞检出率为88.7%,合格率为100%。结论 该方法能够准确、高效的测定中药材中3种汞形态化合物的含量。106批次中药材中的汞存在形态主要是以无机汞为主。

Determination of Inorganic Mercury, Methyl Mercury, Ethyl Mercury in Chinese Herbal Medicine by HPLC-ICP-MS

Objective HPLC-ICP-MS was used to establish the method of simultaneous determination of inorganic mercury, methyl mercury, ethyl mercury in Chinese herbal medicine. To accumulate basic data and provide technical support for Chinese medicine yinpian quality safety regulation, the content of 106 batches of 3 different forms of mercury compounds in Chinese herbal medicine were determined. Methods The sample was extracted by artificial gastric juice in the water bath heating. Methanol-ammonium acetate as the mobile phase, using C18 reversed-phase chromatographic column separation of sample solution, finally the content of three different forms of mercury compounds were determined by ICP-MS. Results The results of three different forms of mercury compounds in 0.5 ~ 5 ng/mL range are good linear relationship, and the correlation coefficient were greater than 0.999.To evaluate the accuracy by the method of standard addition recovery, the recovery is 75.5% ~ 118.0%, RSD was 2.4% ~ 9.7%. In 106 batches of Chinese herbal medicine, methyl mercury and ethyl mercury have not been detected. The detected rate of inorganic mercury was 88.7%, and the percent of pass is 100%. Conclusion The method can accurately and efficiently determinate of the content of three different forms of mercury compounds in Chinese herbal medicine. The main mercury compound of 106 batches in Chinese herbal medicine is inorganic mercury as the existence form.