高效毛细管电泳法测定雄黄微生物炮制液中砷的形态成分

Separation and Analysis of Arsenic Species in Realgar Processing Solution Using Bacteria by CZE

目的建立一种中药复杂体系中砷形态的分离分析方法,确定雄黄炮制液中砷的形态种类和含量。方法以常规炮制雄黄为对照,采用毛细管电泳法测定了3种雄黄微生物炮制液中（iAsⅢ、iAsV、MMAV和DMAV）的含量,其优化条件为：BGE：PDC/10 mmol.L-1和CTAOH/1 mmol.L-1。分离条件：电压25 kV,温度25℃,pH11.0,紫外检测波长设定在216nm。结果雄黄炮制液中4种形态砷能实现完全分离,4种成分的线性范围分别为：iAsⅢ：1.03~513.0 mg.ml-1（r=0.999 8）,iAsV：20~430.2 mg.ml-1（r=0.999 1）,MMAV：1.08~310.3 mg.ml-1（r=0.999 2）,DMAV：1.14~150 mg.ml-1（r=0.999 3）。日内迁移时间和峰面积的相对标准偏差分别为0.61%~0.82%,1.26%~3.12%。回收率范围为97.8%~103.2%。结论该方法较为简便、快速、准确、重现性好,适用于分离测定雄黄炮制液中砷的形态成分分析和其炮制质量控制。.

Objective To establish a new method for separation and determiation of four kinds of arsenic species（iAsIII、iAsV、MMAV and DMAV） in Realgar processing solution by bacteria.Methods Soluble arsenic in Realgar was normal leached by diluted hydrochloric acid（pH 1） or bioleached by special bacteria.Capillary zone electrophoresis（CZE） was used to separate simultaneously and determine quantitatively of four kinds of arsenic species in different leaching solutions of Realgar.The optimum conditions for the determination of active ingredients were as follows：（BGE） containing 10 mmol·L-1 PDC and 1mmol·L-1 CTAOH,voltage 25 KV,working temperature 25°C and detection at 216 nm.Results We first successfully separated iAsIII,iAsV,MMAV and DMAV in different processing solutions.The linear calibration range was 1.03～513.0 mg·ml-1（r=0.999 8） for iAsIII,20～430.2 mg·ml-1（r=0.999 1） for iAsV,1.08～310.3 mg·ml-1（r=0.999 2） for MMAV,1.14～150 mg·ml-1（r=0.999 3） for DMAV respectively.Under the optimum conditions,the relative standard deviation（RSD） values（n = 6） for the migration time and the peak area of each peak were 0.61 %～0.82 %,1.26 %～3.12 %,respectively.The contents of the analytes were easily determined with recovery range from 97.8 %～103.2 %.Conclusion This is a simple,accurate and credible method for analysis of various arsenic species in Realgar processing solution using bacteria.