Page 52 - 理化检验-化学分册 2021年第六期

赵清佳, 等: 在线固相萃取 Ｇ 超高效液相色谱 Ｇ 串联质谱法测定尿液中芬太尼及其代谢物的含量

DeterminationofFentan y landItsMetaboliteinUrineb y
OnＧlineSPECombinedwithUHPLCＧMS MS
/
２
１ , ２
２
１
ZHAOQ in gj ia , WANGRon g XUZhiru , SHENGZhenhai ,
,
２
LIANGChen , ZHANGYuron g ２∗
( １． StateKe yLaborator yo f New Dru gandPharmaceuticalProcess , ChinaState
Instituteo fPharmaceuticalIndustr y , Shan g hai２０００４０ , China ;
２．Shan g haiKe yLaborator yo fCrimeSceneEvidence , Shan g haiInstituteo f
ForensicScience , Shan g hai２０００８３ , China )
Abstract : A methodwasestablishedforthedeterminationoffentan y landits metabolite ( norfentan y l ) in
urineb yonＧlineSPEcombined with UHPLCＧMS / MS , which wasa pp liedtothestud yofdetection window of
－１
fentan y landitsmetaboliteinraturine．Theurinewasdilutedwith２mmol L ammoniumformatebuffersolution
at p H９．２ , andthedilutedsam p lewasdirectl y in j ectedaftercentrifu g ation．Thetar g etcom p oundswereenriched
andp urifiedb yonＧlineSPEwithOasisHLBsolidp haseextractioncolumn , andelutedontotheH yp esilGOLDC １８
anal y ticalcolumnwiththeinitialmobilep haseoftheanal y ticalp um p ．A mixtureofmethanolsolutioncontainin g
－１ －１
φ
２mmol L ammonium formateand０．１％ ( ) formicacid , anda q ueoussolutioncontainin g２ mmol L
ammoniumformateand０．１％ ( ) formicacidindifferentratioswasusedasthemobilep haseforg radientelution．
φ
＋
ESI andthemodeofselectedion monitorin g ( SRM ) wereado p tedin MS / MS．Raturinesam p leswerecollected
－１
afterthetailveinin j ectionfentan y lofratsatadoseof２０ μ g k g , andthedetectionwindowofthe p rotosomeand
metabolitewasstudiedb y thismethod．Asshownb ytheresults , linearrelationshi p sbetweenvaluesofp eakarea
－１
andmassconcentrationoffentan y landnorfentan y lwerefoundinthesameran g eof２．００－８００n g L , withthe
－１
samedetectionlimit ( ３S / N ) of０．２００n g L ．RSDs ( n＝５ ) ofthedeterminedvalueswerealllessthan１５％．The
detectionwindowofp rotosomefentan y linraturinewas５－７d , whilethedetection window ofits metabolite
norfentan y lcouldbeu p to２８d．
Ke y words : UHPLCＧMS / MS ; onＧlinesolidp haseextraction ; fentan y landitsmetabolite ; detectionwindow

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