气相色谱_质谱法同时检测10种常见精神类药物

-10吴惠勤*1　金永春1,2　蔡明招2　黄晓兰1　朱志鑫11(,510070)2(,510640)　　-(GC-MS),10。、GC-MS,、、、、、、、、10。,70.10～25.0mg/L;30.50～25.0mg/L,77%～97%;RSD7%;5～40μg/kg。　-,,,,,PM3　2006-07-20;2006-11-17(No.2004B32401002)*E-mail:[e-mail]1　　、、、、、、、、10,,。,,10,105[1,2]。。,,[3～6]。。、,,5[7～9];[10～13],,,,,。/,10。,、,pH,,/,,。,,,,,、。2　2.1　6890/5973iGC-MS-()。AS3120(AutoScience);PHS-25pH()。、、、、、、、、101.00g/L,4℃,。、、、、、6();、、、4()。、、、()。2.2　10,0.100mg/L。10.0mL,1mL10%(K2HPO4),,;1.00mol/LHClpH1.5。,20mLV∶V=1∶1;15min,3,,3520074　　　　　　　　　　　　(FENXIHUAXUE)　ChineseJournalofAnalyticalChemistry　　　　　　　　　　　　4500～504,1.00mL,。2.3　SPB-1,30m×0.25mm,0.25μm,280℃,150℃,10℃/min290℃;100kPa,He;1.0μL;10∶1。EI,70eV,230℃,GC-MS280℃,150℃,2300V,:29～600amu,:SCAN。3　3.1　-。、、、,∶(5∶5,V/V),,。,,,。,,[14]。,10%[15]。3.1.1　　2.2,、∶(5∶5,V/V)310(pH≈3),31。1　10Fig.1　TICof10drugsextractedbydifferentsolventA.(ether);B.(chloroform);C.∶(methanol∶acetone)5∶5,V/V。1.(nikethamide);2.(lidocaine);3.(phenobarbital);4.(noramidopyrine);5.(atropine);6.(promethazine);7.(carbamazepine);8.(diazepam);9.(chlorpromazine);10.(clozapine)。1,,,,,、、4;,,,10,。,;∶,,,。3.1.2　　,,,。∶(5∶5,V/V),pH1.5、3.55.5(2)。2,,。,,。,pH=1.5。3.2　,。PM3,3。3,N,。,N,,N,(1)。5014:-10　　2　∶(5∶5,V/V)310Fig.2　TICof10drugsextractedinthreedifferentacidmediabymethanol∶acetone(5∶5,V/V)1.(nikethamide);2.(lidocaine);3.(phenobarbital);4.(noramidopyrine);5.(atropine);6.(promethazine);7.(carbamazepine);8.(diazepam);9.(chlorpromazine);10.(clozapine)。　3　PM3Fig.3　Electrondensityintheamidestructureafterparamericmethod3(PM3)optimizationCOR2NHR1+H+N+HHR1COR2(1),N,。,,。3.3　103.3.1　　、、,。,,　4　10Fig.4　TICof10drugsafteroptimization1.(nikethamide);2.(lidocaine);3.(phenobarbital);4.(noramidopy-rine);5.(atropine);6.(prometha-zine);7.(carbamazepine);8.(dia-zepam);9.(chlorpromazine);10.(clozapine)。。,。3.3.2　　30m。15m,10。,,,0.25mm0.25μm,,。,2.3。104。3.4　10,,。,,。,。101。3.5　,10,0.10、0.50、1.00、2.50、5.00、10.025.0mg/L,,Aρ,502　　35,3,2。5～40μg/kg,。1　10Table1　Retentiontimesandcharacteristicionsofthe10drugsDrugs(t/min)Referencestandardsretentiontime(t/min)Sampleretentiontime(m/z)CharacteristicionsNikethamide4.4414.430106,177,78Lidocaine7.9267.91286,58,30Phenobarbital8.5378.525204,117,232Noramidopyrine8.9958.99256,217,83Atropine11.03110.914124,43,289,Promethazine11.85311.83872,180,284Carbamazepine11.91311.899193,236,165Diazepam13.14413.130256,283,221Chlorpromazine13.77313.76058,318,86Clozapine17.31717.310243,256,192　2　10Table2　Linearregressionequationanddetectionlimitofthe10drugsDrugsLinearrange(mg/L)LinearregressionequationCorrelationcoefficients(r)Detectionlimit(μg/kg)Nikethamide0.10～25.0A=2.35×105ρ+0.281x1050.998310.0Lidocaine0.10～25.0A=10.6×105ρ-9.32×1050.999015.0Phenobarbital0.10～25.0A=8.81×105ρ+1.71×1050.998410.0Noramidopyrine0.10～25.0A=0.84×105ρ+3.27×1050.99835.0Atropine0.10～25.0A=0.82×105ρ+3.25×1050.99615.0Promethazine0.50～25.0A=2.25×105ρ+2.18×1050.998240.0Carbamazepine0.10～25.0A=4.84×105ρ+1.65×1050.998720.0Diazepam0.50～25.0A=7.38×105ρ+9.86×1050.993810.0Chlorpromazine0.10～25.0A=3.47×105ρ+2.47×1050.99835.0Clozapine0.50～25.0A=3.49×105ρ+0.612×1050.998640.0　3.6　,,0.100mg/L,GC-MS5,,3。77%～97%,2.65%～6.91%,。3　10Table3　RecoveryandRSDof10drugsDrugsAdded(mg/L)Found(n=5,mg/L)Recovery(%)RSD(%)Nikethamide0.1000.08585.56.91Lidocaine0.1000.08080.25.43Phenobarbital0.1000.07777.25.61Noramidopyrine0.1000.09595.83.90Atropine0.1000.09393.64.28Promethazine0.1000.08585.65.74Carbamazepine0.1000.09797.42.65Diazepam0.1000.08181.75.12Chlorpromazine0.1000.08888.64.81Clozapine0.1000.09292.24.36　5034:-10　　References1　WangHanbin(),NiuWenkai(),ZhangJin(　).ChineseJournalofInternalMedicine(中华内科杂志),2002,41(6):408～4102　SunChengwen(),WangHanbin(),QiuZewu().ChineseJournalofPsychiatry(中华精神科杂志),2001,34(4):239～2413　Teatino,BarbaroA.ForensicScienceInternational,2004,146:93～944　GaillardY,BillaultF,PépinG.ForensicScienceInternational,1997,86:173～1805　CherkaouiS,MateusL,ChristenP,VeutheyJL.J.Pharm.Biomed.Anal.,1998,17(6-7):1167～11766　CherkaouiS,MateusL,ChristenP,VeutheyJL.J.Chromatogr.B,1997,696(2):283～2907　YangGuonong(),ZhuGuofeng().TheChineseJournalofModernAppliedPharmacy(中国现代应用药学杂志),2002,19(4):313～3158　TanLi(　),LiKe(　).JournalofChinaPharmaceuticalUniversity(中国药科大学学报),1994,25(6):328～3319　MoBinbin(),ZhangBikui(),SunYinxiang().ChinesePharmaceuticalJournal(中国药学杂志),2003,38(7):537～53910　FengCuiling().Agro-EnvironmentalProtection(离子交换与吸附),1994,10(2):148～15211　FengCuiling(),LiuYintang(),LuoYi(　).ChineseJournalofPharmaceuticalAnalysis(药物分析杂志),1994,14(5):3～612　BermejoAM,LopezP,AlvarezI.ForensicSci.Int.,2006,156(1):2～813　StaerkU,KulpmannWR.J.Chromatogr.B,2000,745(2):399～41114　WangLiping(),LiXiang(　),SunYing(　).ChineseJ.Anal.Chem.(分析化学),2005,33(7):951～95415　LiangPei(　),QinYongchao(),JiangZucheng().ChineseJournalofAnalysisLaboratory(分析试验室),2000,19(3):56～59SmiultaneousDeterminationof10MentalDrugsbyGasChromatography-MassSpectrometryWuHui-Qin*1,JinYong-Chun1,2,CaiMing-Zhao2,HuangXiao-Lan1,ZhuZhi-Xin11(GuangdongKeyLaboratoryofChemicalEmergencyTest,ChinaNationalAnalysisCenter,Guangzhou510070)2(SouthChinaUniversityofTechnology,CollegeofChemicalScienc