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目的:建立高效毛细管电泳-激光诱导荧光法(high performance capillary electrophoresis-laser induced fluorescence,HPCE-LIF)测定Cu~(2+)和Cd~(2+)含量的方法,并将其应用于中药材人参重金属的检测。方法:Cu~(2+)与Cd~(2+)通过与荧光络合剂异硫氰酸荧光素酯-偶氮乙二胺四乙酸(fluorescein isothiocyanate isomer I-Aminobenzyl ethylene diamine tetraacetic acid,FITCABEDTA)柱前络合后,以熔融石英毛细管柱(75μm×60.2 cm,有效长度50 cm)为分离通道,经1 mol·L~(-1)NaOH溶液调pH至9.3的0.1 mol·L~(-1)硼酸溶液-0.1 mol·L-1SDS溶液(38.5∶61.5)作为缓冲溶液,分离电压25 kV,检测波长520 nm,毛细管温度25℃,自动压力进样5 s。结果:人参样品中Cu~(2+),Cd~(2+)分离效果良好,并且对两者进行了标准曲线、精密度、重复性和加样回收率试验,在1~150,2~200μg·L~(-1)线性关系良好(r>0.999 2),两者精密度RSD均<2.0%,表明精密度良好;两者重复性RSD均<3.7%,表明重复性良好;两者加样回收率分别为103.30%,100.33%,RSD 2.5%,2.8%。结论:采用毛细管电泳-激光诱导荧光法测定中药材人参中特定重金属,方法可行,很好地解决了中药材重金属离子含量低且不易分离的问题,为中药材重金属离子的检测提供一种新的方便快捷准确的方法,并且相信经过不断探索和改进研究,HPCE-LIF法可用于中药材中更多重金属离子的同时检测。
Objective: To establish a method for the determination of Cu 2+ and Cd 2+ by high performance capillary electrophoresis-laser induced fluorescence (HPCE-LIF) Detection of ginseng heavy metals. Methods: Cu ~ (2+) and Cd ~ (2+) were separated by fluorescent complexing agent fluorescein isothiocyanate isomer I-Aminobenzyl ethylene diamine tetraacetic acid (FITCABEDTA) After the pre-column complexation, the fused silica capillary column (75 μm × 60.2 cm, effective length 50 cm) was used as the separation channel and the pH was adjusted to 9.3 with 1 mol·L -1 NaOH solution. 1) boric acid solution-0.1 mol·L-1SDS solution (38.5:61.5) as a buffer solution, the separation voltage of 25 kV, the detection wavelength of 520 nm, the capillary temperature of 25 ° C, automatic pressure injection for 5 s. Results: The results showed that Cu 2+ and Cd 2+ in ginseng samples were separated well, and the calibration curve, precision, repeatability and recovery rate of Cu 2 + and Cd 2 + The linearity of 200μg · L -1 was good (r> 0.999 2). The RSDs of both were less than 2.0%, which showed good precision. The reproducibility of RSD was <3.7%, indicating good reproducibility. The recoveries of samples were 103.30%, 100.33%, 2.5% and 2.8% respectively. Conclusion: The method of capillary electrophoresis with laser-induced fluorescence method for determination of certain heavy metals in ginseng of Chinese herbal medicines is feasible and can well solve the problem of low content of heavy metal ions in traditional Chinese medicine and is not easy to be separated. It provides a new method for the detection of heavy metal ions in traditional Chinese medicine Convenient and accurate method, and believe that after continuous exploration and improvement of research, HPCE-LIF method can be used for the simultaneous detection of more heavy metal ions in Chinese herbal medicines.