仿生提取-高效液相色谱-电感耦合等离子体质谱技术测定冰硼散及朱砂药材中可溶性汞的含量

目的:建立仿生提取-高效液相色谱-电感耦合等离子体质谱技术测定冰硼散及朱砂药材中可溶性汞含量的分析方法,可用于研究冰硼散及朱砂药材的用药安全性。方法:通过模拟人体胃肠道环境,采用人工胃液提取冰硼散及朱砂中的可溶性汞,结合高效液相色谱(以十八烷基硅烷键合硅胶为填充剂;8%甲醇-0.06 mol·L^-1乙酸铵-0.05%2-巯基乙醇的水溶液为流动相;流速0.4 mL·min^-1;进样体积20μL)-电感耦合等离子体质谱技术进行分析测定。结果:通过检测15批冰硼散样品及9批朱砂药材,结果甲基汞、乙基汞、无机汞分别在0.0007~0.28、0.007~1.4、0.17~34 ng·mL^-1范围内,浓度与峰面积呈良好的线性关系,r值分别为0.9997、0.9995、0.9998,平均回收率分别为96.8%、99.7%、98.0%,RSD分别为2.3%、2.8%、5.5%(n=6)。冰硼散中甲基汞含量为0.00046~0.018 mg·kg^-1,无机汞含量为0.64~4.73 mg·kg^-1,乙基汞含量为0.075~0.096 mg·kg^-1;朱砂中甲基汞含量为0~0.034 mg·kg^-1,无机汞含量为8.54~101.07 mg·kg^-1,乙基汞含量为0~0.82 mg·kg^-1。结论:该方法简便、快速、灵敏,重现性好,可用于冰硼散及朱砂药材中可溶性汞的测定。

Determination of Soluble Mercury in Ice Boron Powder and Cinnabar by Bionic Extraction-High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

Objective: A method for the determination of soluble mercury in ice boron powder and cinnabar by bionic extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry was established, which can be used to study the safety of ice boron powder and cinnabar. Methods: By simulating the environment of human gastrointestinal tract, the soluble mercury in ice boron powder and cinnabar was extracted by artificial gastric juice. High performance liquid chromatography (Octadecyl silane bonded silica gel was used as filler. The mobile phase was the aqueous solution of 8% methanol-0.06 mol·L^-1 ammonium acetate-0.05% 2-mercaptoethanol. Flow rate:0.4 mL·min^-1; 20 micron injection volume)-inductively coupled plasma mass spectrometry for analysis and determination. Results: Through the detection of 15 batches of ice boron powder samples and 9 batches of cinnabar medicinal materials, the results showed a good linear relationship between the concentration and peak area of methyl mercury, ethyl mercury and inorganic mercury in the range of 0.0007-0.28, 0.007-1.4 and 0.17-34 ng·mL^-1, r value was 0.9997, 0.9995, 0.9998, respectively. The average recoveries were 96.8%, 99.7% and 98.0%, respectively, and the RSD were 2.3%, 2.8% and 5.5%, respectively (n=6). The content of methyl mercury in ice boran powder was 0.00046-0.018 mg·kg^-1, inorganic mercury was 0.64-4.73 mg·kg^-1, and ethyl mercury was 0.075-0.096 mg·kg^-1. The content of methyl mercury in cinnabar was 0-0.034 mg·kg^-1, inorganic mercury was 8.54-101.07 mg·kg^-1, and ethyl mercury was 0-0.82 mg·kg^-1. Conclusion: The method is simple, rapid, sensitive and reproducible, which can be used for the determination of soluble mercury in ice boron powder and cinnabar.