中药凤尾草不同药用部位的砷形态分析.docVIP

中药凤尾草不同部位的砷形态分析 陈岩1*，王智勇2，杨丽杰1，黄智坤1（1.哈尔滨医科大学第一附属医院药学部，黑龙江 哈尔滨 150001；2. 哈尔滨医科大学第二附属医院静脉药物配制中心，黑龙江 哈尔滨 150086） [摘要] 目的：建立凤尾草中砷化合物的分析方法。方法：用高效液相-原子荧光光谱联用方法，以KH2PO4/Na2HPO4的缓冲溶液为流动相（pH 5.90），采用等度洗脱方式，用Hamilton PRP-X100阴离子交换色谱柱（250 mm×4.1 mm，10 μm），流速1.2 mL·min-1对不同方法提取的凤尾草中的亚砷酸根（AsO33-）、砷酸根（AsO43-）和一甲基砷（MMA）、二甲基砷（DMA）进行分离，进样量10μL，原子荧光光谱仪在线检测。结果： AsO33-和AsO43-线性范围为2.5 ng · mL-1~ 25 ng · mL-1（r＝0.999 8），日内、日间精密度（RSD）均小于2.5%，平均回收率在96.92%-102.31%之间。50%甲醇为提取溶剂，室温下超声波提取3批凤尾草中的砷化物，叶中含量最高，根中含量次之，茎中含量最低。结论：本研究改进了中药中各种形态的砷化合物的提取和分析方法，操作简便，灵敏度高，结果准确，重现性好，为中药中各种形态的砷化合物分析方法提供了新的依据和方法。 [关键词] 凤尾草；砷形态分析；高效液相色谱法；原子荧光光谱法 Speciation Analysis for Arsenic in different medicative parts of Chinese Crude Drug Pteris multifida Poir CHEN Yan1, WANG Zhi-yong2，YANG Li-jie1, Huang Zhi-kun1（1. Dept. of Pharmacy，The First Affiliated Hospital of Harbin Medical University，Heilongjiang Harbin 150001，China；2. Pharmacy Intravenous Admixture Services，The Second Affiliated Hospital of Harbin Medical University，Heilongjiang Harbin 150086，China） [ABSTRCT] OBJECTIVE：To establish the speciation analysis for arsenic in Chinese crude drug Pteris multifida Poir. METHODS：The arsenic speciations in Pteris multifida Poir（PMP） were determinated by HPLC-AFS on Hamilton PRP-X100 anion exchange column（250 mm×4.1 mm，10 μm），using KH2PO4/Na2HPO4 buffer solution（pH 5.90）as moble phase at room temperature and a flow rate was 1.2 mL·min- 1. RESULTS：The linear concentration ranges of the calibration curves for AsO33- and AsO43- were from 4.0 ng·mL- 1 to 40.0 ng·mL- 1（r＝0.999 8）. The intra- and inter-day precision（RSD）were less than 2.5%. The recoveries ranged from 96.92%-102.31%. 50% methanol as solvent, at room temperature under ultrasonic extraction of 3 batches of PMP, the highest content of arsenic was in leaves, followed by the content of the root, the stem was the lowest. CONCLUSION：This study improved the extraction and analytical methods of arsenic in traditional Chinese medicine compounds, which were simple ope