LC_MS_MS法快速测定中成药_保健食品中非法添加的36种化学成分

LC-MS/MS36*李丹1,文红梅2,崔福春1,黄亚1,郭春1,孙夏荣1,杨婧平2(1.210015;2.210029):36:-(LC-MS/MS),SunfireTMC18(21mm100mm,50m),-01%(7525),(ESI)(MRM),36:36,20ng:,:;;;:R917:A:0254-1793(2010)08-1527-06LC-MS/MSscreeningfor36chemicalcomponentsinhealthfoodandChinesetraditionalpatentmedicine*LIDan1,WENHong-mei2,CUIFu-chun1,HUANGYa1,GUOChun1,SUNXia-rong1,YANGJing-ping2(1.NanjingInstituteforDrugContro,lNanjing210015,China;2.NanjingUniversityofTraditionalChineseMedicine,Nanjing210029,China)AbstractObjective:Toestablishaliquidchromatography-tandemmasschromatography(LC-MS/MS)methodforthesimultaneousscreening36chemicalcomponentsinhealthfoodandChineseTraditionalPatentMedicine.Methods:Thismethodinvolvesliquidchromatography-tandemmassspectrometry,theseparationwasconductedbySunfireTMC18(21mm100mm,50m).Themobilephaseconsistedof01%formicandmethanol(2575).ThetargetcompoundswereanalyzedwithLC-MS/MS-ESI.Multiple-reactionmonitoring(MRM)wasusedtoscreen36chemicalcomponentsinhealthfoodandChineseTraditionalPatentMedicine.Results:Afastandsensitiveliquidchromatographymassspectrometric(LC/MS)methodforthesimultaneousscreeningof36chemicalcomponentswasdescribed.TheLODofthesesubstanceswerebelow20ng.Conclusion:ThemethodwassufficientlyselectiveandsensitivetodetectchemicalcomponentsinhealthfoodandChineseTraditionalPatentMedicine.Keywords:LC-MS/MS,multiple-reactionmonitoring(MRM),chemicalComponents,rapiddetermination,,,,,,,,(2006006)2,,,[1][2],[3,4],36,1111200LLC-MS():,(ESI),,MsworkstationVersion66!1527!ChinJPharmAnal2010,30(8)*2008(200801069)Te:l(025)85036223;E-mai:[e-mail];SartoriusBP211D(Sartorius)12:(10034-200302),(2058-9501),(10198-002),(100679-200401),(100179-200303),(100272-199701),(100487-200301),(10337-0001),(100415-200301),(100667-200401),(100335-200001),(100428-200401),(100364-200301),(100145-199501),(100555-200501),(100353-200301),(100190-200402),(100177-199802),(100503-200301),(0106-9702),(0113-0101),(0002-9504),(100018-200408),(100506-200301),(100525-200301),(0225-9601),(100095-198904),(100394-200401),(100527-200401),(100385-200401),(111616-200301),(100452-200301),(100530-200501),(100547-200401),(100312-200001),(100677-200401),,:(:20081001)221:10mg,,50mL,,,:,50mL,,,22,(1),50mL,,15min,,,,10,045m23SunfireTMC18(21mm100mm,50m)(Waters);-01%(7525);:5L24(ESI);;(MRM);:5kV;407kPa:;:250∀;:138kPa;:2mtorr;:15kV;:05s;Q1:calibration;Q3:calibration255L,LC-MS/MS26(1),,33136(200g#mL-1)1g#mL-1,ESI,,,(DP),(CE)[4](MRM)132:--10mmol-01%,:-01%(7525),-:20mm,5m,C18,10~15cm33,,S/N=3,,5,LC/MS,RSD%,5L,,2,(Y)(X),n16,,2!1528!ChinJPharmAnal2010,30(8)136Tab1Resultof36chemicalcomponentsatMSoptimization(compound)DP(V)(qualitativeion)CE(eV)tR/min(diclofenac54296/214286267sodium)296/25010296/2785296/17945*296/25012(indometacin)65358/139166151358/17410(naproxen)40231/185103391231/17024231/14145231/15330(meloxicam)70352/115144336352/14118(ibuprofen)55207/16186725207/10518207/11920(auranofin)15679/1691952257679/499125679/10926679/215315(feprazone)50321/265114380321/25395321/21119321/13221(ketoprofen)65255/209952990255/105175255/77375255/19419(fenbufen)30255/237753415255/181215255/152405255/20916*(etodolac)90286/242156065286/211235(sulinclac)110357/2332752681357/34016357/248315357/24723(methocarbamol)55264/11881713264/1995264/16310*(chlorzoxazone)65168/132202438168/7628(phenprobamate)35180/91952404180/1195180/1375*(nimesulide)65307/229152865307/227195307/19828307/79215(oxaprozin)75294/103244871294/276125294/234165294/206185(mefenamicacid)35242/22410510377242/20925242/180395(piroxicam)70332/951627241(compound)DP(V)(qualitativeion)CE(eV)tR/min332/12118(aminophenazone)55232/113951466232/111115232/98145232/7019*(salicylicacid)40137/93163960137/6528137/7530*(aspirin)40179/137501946179/9320(metamizolesodium)30310/1911211149310/175225310/176175310/8026(paracetamol)55152/110121574152/93205152/6528(phenazone)70189/77331643189/13116189/147155189/1042170231/1891552316(propyphenazone)231/20119231/146205(benorilate)30314/27252141314/12113314/152165314/1635(phencetin)70180/110182001180/138115(ethenzamide)60166/14961910166/12114166/9324166/131135(lysine35147/84141126acetylsalicylate)147/1305(hilieidum)35285/12381523285/9526*(taurine)70124/79181474124/107125(rolundine)80356/192241113356/165225(bulleyaconitine)120644/1354501115644/584285(lappaconitine)140585/162361115585/32432585/38829(pizotifen)85296/96131133296/19917(benzbromarone)85425/27918519987425/17319425/251375(note):*,(representnegativeion,othersarepositiveions)!1529!ChinJPharmAnal2010,30(8)236Tab2LOD,precisioncalibrationcurversandrecoveryof36components(compound)(LOD)/g#mL-1(precision)/%tR(area)(linearityrange)/g#mL-1(regressioneqution)r(recovery)(n=6)/%(diclofenacsodium)004140587(024,480)Y=1913107X-1401106099881063(indometacin)002099635(027,1071)Y=5152106X-5259105099791028(naproxen)39090307(527,2633)Y=2178106X-146310609969996(meloxicam)002059237(050,494)Y=9694106X+2161106099951021(ibuprofen)20088290(570,4556)Y=2375106X-3681106099951009(auranofin)004071344(050,499)Y=8934105X+238610509979937(feprazone)009139663(028,1105)Y=3981106X-5604105099