LC/TOF-MS MS ( )
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- としはる わくや
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1 LC/TOF-MS MS ()
2 (TOF-MS) MS) LC/MS 1. 2.
3 Agilent 1100 LC/TOF-MS MS ~0.25ppm / C ambient
4 Compound Exact mass Positive Negative Purine TFA Hexakis(1H, 1H, 3H ) -tetrafluoropropoxy) ) Phosphazene ) TO F TOF 1) Formate adduct ion 2) Acetatee adduct ion 3) TFA adduct ion
5
6 LC/TOF-MS MS HPLC Column : Agilent-1100 : Zorbax Eclipse XDB C18 (150mm,2.1mm,5um) Mobile phase : A:ACN B:10mMCH 3 COONH 4 5%A/B---(30min)---100%A/B Column temp : 40C Sample volume : 10ul Flow rate : 0.2ml/min MS : Agilent-1100MSD TOF Ionization : ESI(Positive) Scan range : m/z 100- Lock mass : m/z=121,922 Transient : Drying gas : 9l/min at 350 Nebulizer gas : 50psi Fragmentor : 100V Vcap : 4000V
7 Intensity, cps Dimethyl pthalate Diethyl pthalate 3.Diallyl pthalate 4.Dipropyl pthalate 5.Diisobutyl pthalate 6.Dibutyl pthalate 7.Dihexyl pthalate 8.Diheptyl pthalate 9.Dioctyl pthalate 10. Di2-ethylhexylpthalate : 121:700000cps,922:150000cps : 121:100000cps,922:40000cps : 121: 40000cps,922:15000cps Time, min TIC
8 1ppm 0.1ppm
9
10
11
12 m/z= m/z= Intensity, cps Time, min (500 )TIC, TIC,
13 ppm -3.2ppm ppm (CH2CH2O) Mass error -6.5ppm -7.6ppm -19.5ppm 13.5ppm m/z, amu 1
14 Intensity, counts m/z, amu 1
15 (M+H) Mass error :4.14ppm (2M+H) m/z, amu Intensity, counts m/z, amu (M+H) + Mass error :0.26ppm C13H25N2O (2M+H) m/z, amu Intensity, counts m/z, amu
16 N- LC/TOF-MS MS HPLC Column : Agilent-1100 : Zorbax Eclipse XDB C18 (150mm,2.1mm,5um) Mobile phase : A:ACN B:10mMCH 3 COONH 4 20%A/B---(30min)---100%A/B Column temp : 40C Sample volume : 10ul Flow rate : 0.2ml/min MS : Agilent-1100MSD TOF Ionization : ESI(Positive) Scan range : m/z 100- Lock mass : m/z=121,922 Transient : Drying gas : 9l/min at 350 Nebulizer gas : 50psi Fragmentor : 100V Vcap : 4000V 1.Oxamyl 2.Methiocarbsulfoxide 3.Methiocarbsulfone 4.Aldicarb 5.Bendiocarb 6.Pirimicarb 7.Ethiofencarb 8.Fenobcarb 9.Methiocarb
17 N- (0.5ppb) m/z= m/z= m/z= Intensity, cps m/z= m/z= m/z= m/z= m/z= Time, min Time, min
18 - 1.Oxamyl 2.Methiocarbsulfoxide 3.Methiocarbsulfone 4.Aldicarb 5.Bendiocarb 6.Pirimicarb 7.Ethiofencarb 8.Fenobcarb 9.Methiocarb
19 1 2 Intensity, cps Oxamyl 2.Methiocarbsulfoxide 3.Methiocarbsulfone 4.Aldicarb 5.Bendiocarb 6.Pirimicarb 7.Ethiofencarb 8.Fenobcarb 9.Methiocarb Time, min N- (20ppt ppt)
20 cps cps 20% 20%. ESI ESI 3ppm 3ppm. CID CID 6ppm ppm. 4 3ppm ppm 1~7 1~7. N- ;0.1~1 ;0.1~1ppb ppb ;0.999 ;0.999 ;2.3 ; % 10.1%
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