ICP-MS 研究中药炮制前后18 种微量元素总量和溶出特性的变化.pdf

:rS5(b2009B032)；3D)5(BJnull2008null117)Te:f,3,pVnullZ_:0snullnull*YT:,3,0=nullnullZ_:D0nullnullTe:l(010)85133636nullnullEnullmai:lhuxinbjyy126nullcomICPnullMS0-189+M金鹏飞1,宋丽洁2,胡欣1*,邹定1,吴学军1,孙春华1(1null3D0,100730；2nullS/?Z,102206)K1:null应用电感耦合等离子体质谱(ICPnullMS)技术对中药炮制前后18种微量元素的总量及溶出特性的改变进行考察bZEnull应用ICPnullMS技术建立中药中18种元素的同时测定方法,并用该方法对黄芪a大黄a黄芩a何首乌a地黄等5种中药材炮制前后元素总量和水煎过程中溶出特性的改变进行比较和分析bTnull测定方法中所有元素的线性相关系数(r)都大于0null9990,检出限在0null00010null0689nullgnullL-1之间,重复性和稳定性的相对标准偏差(RSD)都小于10%,药材的加标回收率在70null89%122null4%之间,水煎液的加标回收率在74null65%130null0%之间,标准物质茶叶(GBW07605)的测定值和其标定值之间有良好的吻合性b测定结果显示,炮制后,微量元素总量的变化因中药品种和炮制方法而异,但各元素的溶出率总体呈现上升的趋势bnull中药炮制可改变微量元素的总量和溶出特性b1oM:电感耦合等离子体质谱；中药；炮制；微量元素ms|:R284nullnullnullDS:AnullnullnullcI|:1001-2494(2010)12-0893-05EffectofProcessingonContentandDissolutionof18TraceElementsinTraditionalChineseMedicinesbyICPnullMSJINPengnullfei1,SONGLinulljie2,HUXin1*,ZOUDing1,WUXuenulljun1,SUNChunnullhua1(1nullPharmaceuticalScienceDepartment,BeijingHospital,Beijing100730,China；2nullBeijingHuaxipharmConull,Ltd,Beijing102206,China)ABSTRACT:OBJECTIVEnullToinvestigatecontentanddissolutionfeaturechangesof18traceelementsincrudeandprocessedtradinulltionalChinesemedicines(TCMs)byinductivelycoupledplasmamassspectrometry(ICPnullMS)nullMETHODSnullAnICPnullMSmethodforsimultaneousdeterminationof18traceelementsinTCMswasestablished,andthecontentsanddissolutionfeaturesof18traceelementsin5crudeandprocessedTCMs,RadixAstragal,iRadixetRhizomaRhe,iRadixScutellariae,RadixPolygoniMultifloriandRadixRenullhmanniae,werecomparedandanalyzednullRESULTSnullThevalidatedmethodindicatedthatthecorrelativecoefficients(r)forallelenullmentswereabove0null9990nullThelimitsofdetectionswereintherangeoffrom0null0001to0null0689nullgnullL-1nullThereproducibilityandstabilityweresatisfactorywithallRSDsbelow10%nullThespikedrecoveriesforTCMswerebetween70null89%and122null4%nullThespikedrecoveriesfortheirwaterextractsolutionsrangedfrom74null65%to130null0%,thedeterminedvaluesofteareferencematerial(GBW07625)wereinaccordancewiththosecertifiednullThechangesofelementcontentsdependedontheTCMspeciesandprocessingmethnullods,whilethedissolutionrateofelementsweregenerallyincreasedafterprocessingnullCONCLUSIONnullProcessingTCMcouldchangeitscontentsanddissolutionfeaturesofelementsnullKEYWORDS:ICPnullMS；traditionalChinesemedicine；process；traceelementnullnull0r,A$b,YsT00r$,7s5$bCD0?Z,M00rV?mssxT1null2byN,0c,00r$1ilbD01+b0V,0a0raZ?3M,4U$?3MbI0-c,$M1INbXg0.d0ZTb0XA8=,yN,IXV+0$91ilbL08(ICPnullMS)/,y0MgaAlaVaCraMnaFeaCoaNiaCuanull893nullS02010M64512nullnullnullnullnullnullnullnullnullnullnullnullnullnullChinPharmJ,2010June,Volnull45Nonull12ZnaAsaSeaMoaCdaSnaBaaHgaPb18HZE,iZEavaana50-c+d,t0$4Ib1nullNk008N(ICPnullMS):Agilent7500a(AgilentTechnologiesConullLtd,USA),Babington,|bWX-4000eoyhd(Z)sNK)bB)d(ESMILLIPORE,Synthenullsis)bMETTLERTOLEDOXP2050?(+)b101A-22Q(ZLN9)bRT-02Ax(?/K)bMgaAlaVaCraMnaFeaCoaNiaCuaZnaAsaSeaMoaCdaSnaBaaHgaPbSA,i1000mgnullL-1,(1SESbS:SEB)S=(|02163,oo)bA:L,iY,Ce,T,lCoA(null=10nullgnullL-1),Agilent,I|5184null3566b=SA:Agilent=SA(6Lia45Sca72Gea89Ya115Ina159Tba209B,inull=10mgnullL-1),I|5183null4680bib(MOS)30%H2O2(sB)bB(MILLIPOREBd)b2nullZnullE2null1nullICPnullMS工作参数RFq:1300W；:7null8mm；:1null12Lnullmin-1；,:6rnullmin-1；i:2；Z:EPA200null8；T:Specnulltrum,；:187=S；sHW:0null1s,Q:3Q；-,46:18rnullmin-1,46HW:30s；-,:6rnullmin-1,HW:35sb2null2null中药样品(:,；0K,|:06011704)；v(:,K3,|:601000032)；(:=,K3,|:601000325)；n(:,；0h,h,|AM20mLY,B,(,b2null6null内标溶液的制备|Agilent=SAa,8s10%bA)di0null1mgnullL-1A,(,b2null7null供试品溶液的分析测定和计算N=S5S=SA,GQ|N5iSA(bA),Bi3Q(:US,MiUSTSwLb|5kA,|3Q(,SwL,9Mib3nullT)3null1null方法学验证3null1null1nullL_Knull=S91:US,iUS,18SwL,iILM1(r)brv0null9990(V3)bZE_K/T9:_K(nullgnullL-1)=3/(S-B)nullbT:bA9S(n=11)；nullSAi；SBsYSAbA9b_K1nullgnullL-1/(V3)b3null1null2nullnullL#XAVIZEb|x0null2g(XA0null4g),#2null5/?T,L5z,9c(#RSDbL3d,93d=c(RSDbRSDl10%,z(V3,4)b3null1null3nullFlqnullL#XAVIFSlqb|x0null2g(XA0null4g)h7,i7Fa%!Aa,#2null5/?T,L5z,FS-c(9lq(V4)b0lq70null89%122null4%W,XAlq74null65%130null0%WbV2null供试品的消解程序Tabnull2nullMicrowavedigestionprocedureforsamplesStepsTempnull/Presnull/kPaHoldtime/min1601null01103521001null21103531501null521031042002null0310310V3null18种微量元素线性a检出限和稳定性nulln=3Tabnull3nullLinearity,LOD,andstabilityof18traceelementssnulln=3ElementInternalisotopeCalibrationcurverrLOD/nullgnullL-1Stability(RSD/%)24Mg6LiY=11null10null-11370null99990null06892null2427Al6LiY=8null204null-85null090null99990null00251null5051V72GeY=0null533null-0null2770null99990null00026null4053Cr45ScY=25null82null-0null2670null99980null00264null6755Mn45ScY=4null000null-9null8090null99940null00053null1957Fe45ScY=191null2null-288null70null99930null01902null7559Co45ScY=3null534null-0null1390null99970null00073null4560Ni72GeY=15null74null-0null8490null99980null00032null3563Cu72GeY=1null193null-0null6740null99990null00161null4166Zn72GeY=8null242null-16null580null99900null00285null4675As72GeY=6null623null-0null0780null99990null00116null3382Se72GeY=101null9null-2null5450null99970null01494null3695Mo89YY=19null89null-0null4850null99960null00022null64111Cd115InY=37null01null-0null0070null99930null00024null37118Sn115InY=11null60null-0null1801null00000null00033null60137Ba159TbY=44null53null-18null790null99930null00022null67202Hg209BiY=16null57null-0null0600null99930null00302null24208Pb209BiY=7null574null-0null8090null99950null00011null48null895nullS02010M64512nullnullnullnullnullnullnullnullnullnullnullnullnullnullChinPharmJ,2010June,Volnull45Nonull12V4null18种微量元素重复性和准确度Tabnull4nullReproducibilityandaccuracyof18traceelementElementReproducibilityRSD/%Recovery/%TeareferencematerialTCMWaterextractTCMWaterextractCertified/nullgnullg-1(n=5,x!s)Found/nullgnullg-1Mg4.022.24107.8112.71700!2001650Al3.59UD93.56108.030001)2260V3.785.3977.99102.50.861)0.85Cr3.805.9170.8986.630.8!0.030.828Mn4.322.8686.4574.651240!701224Fe3.42UD92.78113.6264!15250Co4.954.2790.53113.90.18!0.020.16Ni4.412.1496.69111.34.6!0.54.7Cu4.073.2385.2797.3617.3!1.819.0Zn5.453.4185.8895.3426.3!2.024.7As5.375.2995.51130.00.28!0.040.26Se8.367.51102.8101.10.0721)0.118Mo7.034.0480.25104.40.038!0.0070.041Cd6.076.6778.1886.030.057!0.0100.052Sn4.036.8996.06107.8ND0.281Ba7.57UD122.4125.258!655Hg8.908.5079.54114.40.0131)0.021Pb2.394.7283.63101.04.4!0.34.3:UD-_；ND-?；1)A,lV,Se,HgcINote:UD-undetectable；ND-notdefined；1)ThevaluesforA,lV,Se,Hgwerenotcertifiedvalues,butreferencevalues3null1null4nullSnullSEB)S=(GBW07605)ZEBb|S=0null2g,#2null5/?T,L5z,9c(V4)bS?S=b3null2null样品测定及结果分析yZEavaana50cMX+bL5z(n=5),|(bTnV5,6b18,AsaCdaHgaPbaCu8v,SE?g05Kc?b%0#4sS&?4:g0#4Asc2nullgnullg-1,Cdc0null3nullgnullg-1,Hgc0null2nullgnullg-1,Pbc5nullgnullg-1,Cuc20nullgnullg-1bVavaana0#TA,5c1pbn,+cC9；,cC9；v,c9M；7,cC/b4U,0,c?3M,0,ZE,Mt9MbD5null6,-cMV?0WM1:c9F,0t()；ch,0te()bL0K,y79EBbV+A:(AlaVaCraFeaBaq,4UtV?i,9V?sb)NiaCuaZnaSeaMoqYv,4Ut0iTbHgaCuY,qC6；,q6q/；vn,q9Mb,0,q98C6tbnull896nullChinPharmJ,2010June,Volnull45Nonull12nullnullnullnullnullnullnullnullnullnullnullnullnullS02010M64512V5null元素总量测定结果nullnullgnullg-1Tabnull5nullResultsofelementcontentsnullnullgnullg-1ElementRadixAstragaliRadixetRhizomaRheiRadixScutellariaeRadixPolygoniMultifloriRadixRehmanniaeCrudeProcessedCrudeProcessedCrudeProcessedCrudeProcessedCrudeProcessedMg162012262808165448435775732949925882Al24613930057987339999.4169765744V0.390.220.400.851.910.820.100.261.191.24Cr2.621.122.204.494.342.660.951.613.054.82Mn13.79.4727.915.322.516.17.559.7313.515.4Fe27427834758166332471.3195570631Co0.210.120.220.300.500.290.100.160.330.38Ni2.791.932.174.332.871.500.621.362.133.41Cu5.654.764.052.937.227.823.044.032.783.52Zn24.629.615.28.8313.313.510.022.98.9113.7As0.150.101.280.370.470.100.040.110.810.52Se0.120.040.560.250.070.030.010.030.670.83Mo3.605.410.090.050.040.130.060.280.030.02Cd0.030.010.090.050.020.020.030.040.030.02Sn0.040.040.060.200.070.060.100.060.090.10Ba5.852.8612968.960.364.64.969.049.729.84Hg0.050.040.060.040.100.100.020.030.030.01Pb0.470.390.510.870.920.920.480.721.181.53V6null元素溶出率测定结果null%Tabnull6nullResultsofelementdissolutionratesnull%ElementRadixAstragaliRadixetRhizomaRheiRadixScutellariaeRadixPolygoniMultifloriRadixRehmanniaeCrudeProcessedCrudeProcessedCrudeProcessedCrudeProcessedCrudeProcessedMg56.583.166.780.768.365.647.689.369.470.3AlUD1.1716.310.80.910.687.4519.45.079.67V4.727.603.931.781.400.538.982.326.1017.5Cr16.926.620.612.47.9915.321.922.313.59.88Mn38.855.837.850.333.648.158.774.743.043.5FeUD8.525.9615.21.332.158.6615.317.921.2Co41.454.244.029.421.636.947.968.842.947.4Ni57.571.974.730.617.620.875.751.841.222.4Cu82.356.358.242.729.137.984.045.057.761.3Zn37.438.790.994.638.966.710488.569.866.5As52.482.578.590.159.174.487.489.478.482.9Se35.346.413.45.2025.582.584.767.023.023.4Mo10584.37.895.269.506.2717.39.5384.577.0Cd23.446.528.145.320.033.526.543.326.638.7Sn73.878.284.029.663.576.782.788.154.442.6BaUDUD3.854.7928.236.729.848.214.611.5Hg37.623.376.620.047.434.561.121.143.054.5Pb37.466.636.665.236.850.953.238.719.231.0:UD-_Note:UD-undetectableREFERENCES1nullCHAOZQnullRecentprogres