雄黄及制剂中砷含量测定与形态分析

Content determination and speciation analysis of arsenic in realgar and its compound preparations

目的:应用原子荧光光谱法(AFS)和液相色谱-原子荧光联用法(HPLC-AFS)对雄黄及5种不同处方含雄黄复方制剂中总砷含量、可溶性砷含量、可溶性砷的形态进行研究,为含雄黄药品质量安全评价提供参考。方法:样品经微波消解后,采用原子荧光光谱法测定样品中总砷含量。可溶性砷经模拟人工胃液振荡提取、甲醇-水(1∶1)超声提取2种方法提取后,采用原子荧光光谱法测定样品中可溶性砷含量,用高效液相色谱-原子荧光联用法分析样品中各形态砷化合物并测定其含量。结果:原子荧光光谱法线性范围为0~10μg·L^-1,总砷加标回收率为94.0%,RSD 2.2%;可溶性砷加标回收率96.4%~96.5%,RSD 1.9%~7.7%。液相色谱-原子荧光联用法线性范围为0~100μg·L^-1。甲醇超声提取方法各价态砷的回收率在84.9%~101.2%之间,RSD 2.5%~8.2%,人工胃液振荡提取方法各价态砷的回收率在83.2%~93.8%之间,RSD 2.3%~7.2%。雄黄及其复方制剂中可溶性总砷含量仅占样品总砷含量的0.26%~1.05%;所有样品中检测出来的砷形态只有As(Ⅲ)和As(Ⅴ)。结论:联合运用原子荧光光谱法、液相色谱-原子荧光联用法可测定雄黄及其复方制剂中总砷、可溶性砷及砷形态分析。

Objective:To study arsenic,soluble arsenic and the speciation of soluble arsenic in realgar and 5 kinds of compound preparations by AFS and HPLC-AFS, and provide reference for evaluation of quality and safety of realgar-containing drugs. Methods:After microwave digestion,the total arsenic content in samples was determined by atomic fluorescence spectrometry. After artificial gastric fluid oscillation extraction or methanolwater(1∶1) ultrasonic extraction,determine the content of soluble total arsenic in samples by atomic fluorescence spectrophotometry. Analyze the speciation of arsenic and determine its content by high performance liquid phaseatomic fluorescence. Results:The linear relationship was good in the range of 0-10 μg·L^-1 in AFS,The recovery of standard addition was 94.0% in arsenic,RSD 2.2%. The recovery of standard addition in soluble arsenic was 96.4%-96.5%,RSD 1.9%-7.7%. The linear relationship was good in the range of 0-100 μg·L^-1 in HPLC-AFS. 84.9%-101.2% by methanol-water(1:1) ultrasonic extraction,RSD 2.5%-8.2%;83.2%-93.8% by artificial gastric fluid oscillation extraction,RSD 2.3%-7.2%. The content of total soluble arsenic in realgar and its compound preparations accounted for only 0.26%-1.05% of total arsenic in the sample. Arsenic species detected in all samples were As(III) and As(V) only. Conclusion:AFS and HPLC-AFS are suitable to the detection of the arsenic,soluble arsenic and speciation of soluble arsenic in realgar and 5 kinds of compound preparations.