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1、第28卷第8期分析测试学报Vol128No182009年8月FENXICESHIXUEBAO(JournalofInstrumentalAnalysis)918~92115种中药材中砷的形态分析1,23212郝春莉,王庚,余晶晶,陈曦,王小如(1.厦门华厦职业学院食品药品安全检测中心,福建厦门361024;2.国家海洋局第一海洋研究所现代分析技术及中药标准化重点实验室,山东青岛266061;3.防化研究院,北京102205)摘要:利用高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)联用技术对6种砷形态[砷胆碱
2、(AsC)、砷甜菜碱(AsB)、三价砷As(Ⅲ)、二甲基砷酸(DMA)、甲基砷酸(MMA)和五价砷As(Ⅴ)]进行了2分离,测定了0~100μg/L范围内6种砷形态的混合标准工作曲线,相关系数(r)优于01990,方法检出限均为012μg/L。采用甲醇-水(体积比1∶1)超声法提取了15种中药材中的砷形态,用HPLC-ICP-MS进行分析,结果表明,15种中药材中存在的主要砷形态是有毒的As(Ⅴ),另外还有少量的砷甜菜碱和砷胆碱,并且动物用药中的有机砷含量明显高于植物用药。关键词:砷元素;砷形态分析;高效液相色谱-电感耦合
3、等离子体质谱;中药材中图分类号:O657163;TE622113文献标识码:A文章编号:1004-4957(2009)08-0918-04doi:1013969/j1issn11004-4957120091081009ArsenicSpeciationAnalysisof15TraditionalChineseMedicines1,23212HAOChun2li,WANGGeng,YUJing2jing,CHENXi,WANGXiao2ru(1.TestingCenterforFoodandDrugSafety,Xiame
4、nHuaxiaVocationalCollege,Xiamen361024,China;2.QingdaoKeyLabofAnalyticalTechnologyDevelopmentandStandardizationofChineseMedicines,FirstInstituteOceanographyofStateOceanicAdministration,Qingdao266061,China;3.ResearchInstituteofChemicalDefense,Beijing102205,China)Abs
5、tract:Thehyphenatedtechniqueofhighperformanceliquidchromatographycoupledwithinduc2tivelycoupledplasma2massspectrometry(HPLC-ICP-MS)wereappliedinthesimultaneousdeter2minationofsixarsenicspeciesincludingAsC,AsB,As(Ⅲ),DMA,MMAandAs(Ⅴ),in15traditionalChinesemedicines(T
6、CMs).Sixmixedarsenicstandardswereusedforthemethodevalua2tion.Theexperimentalresultsshowedthatthecalibrationcurveswerelinearintheconcentrationrangeof0-100ng/gwithcorrelativecoefficientsmorethan01990.Thedetectionlimitsforsixspe2cieswere012μg/L.Thearsenicspeciesinthe
7、seTCMswereextractedusing1∶1(byvolume)methanol-H2O,andweredetectedwithmethodmentionedabove.Theresultindicatedthatthemaininorganicformsofarsenicwerepresentedinthesemedicinesandasmallquantityofnon2toxicarsenobetaineandarsenocholinewerefound,inwhichtheconcentrationofo
8、rganicarseniccompoundsexistedinanimalherbswashigherthanthatofplantones.Thisfeasiblemethodisanimportantmeth2odologyforthetoxicologicresearchofAs,andcould