LC/TOF-MS MS ()
(TOF-MS) MS) LC/MS 1. 2.
Agilent 1100 LC/TOF-MS MS ~0.25ppm / C ambient
Compound Exact mass Positive Negative Purine 121.050873 TFA 112.985587 Hexakis(1H, 1H, 3H 922.009798 966.000725 1) -tetrafluoropropoxy) 980.016375 2) Phosphazene 1033.988109 3) TO F TOF 1) Formate adduct ion 2) Acetatee adduct ion 3) TFA adduct ion
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 : 10000 Drying gas : 9l/min at 350 Nebulizer gas : 50psi Fragmentor : 100V Vcap : 4000V
Intensity, cps 10 6 7.0 1.Dimethyl pthalate 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 2.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 1 2 2 3 3 4 6 5 7 8 910 : 121:700000cps,922:150000cps : 121:100000cps,922:40000cps : 121: 40000cps,922:15000cps 8 9 10 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 Time, min TIC
1ppm 0.1ppm
10 6 3.4 m/z=399.2-399.33 10 7 2.8 2.2 m/z=364.2-364.3 1.8 1.6 Intensity, cps 1.6 1.4 1.2 1.0 0.8 1.0 4.0 24.2 24.6 25.0 25.4 25.8 26.2 0.6 0.4 0.2 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 Time, min (500 )TIC, TIC,
120000 110000 100000 90000 80000 70000 60000 50000 40000 30000 20000 10000 460.24096 504.26638 548.29245 592.31787 636.34381 680.37036 724.39565 768.42251 812.44668 856.47437 358.20665 314.18033 460.24096-18.5ppm -3.2ppm 504.26638 548.29245-18.2ppm 592.31787 636.34381 680.37036 724.39565 44.02594(CH2CH2O) Mass error -6.5ppm -7.6ppm -19.5ppm 13.5ppm 768.42251 812.44668 856.47437 150 250 350 450 550 650 750 850 950 m/z, amu 1
100000 90000 416.21585 460.24037 402.23271 446.25886 490.28502 534.31254 578.33862 504.26654 548.29242 Intensity, counts 80000 70000 60000 50000 40000 592.31783 437.25371 402.23271 446.25874 393.22738 358.20662 490.28502 534.31165 578.33709 30000 20000 10000 340 360 380 400 420 440 460 480 500 520 540 560 580 600 m/z, amu 1
171.14986(M+H)+ 10 6 Mass error :4.14ppm 10 5 1.0 0.8 0.6 0.4 0.2 341.29061(2M+H) + 120 150 180 210 240 270 300 330 m/z, amu Intensity, counts 7.0 5.0 3.0 1.0 364.26918 399.25085 120 160 200 240 280 320 360 400 440 m/z, amu 10 5 7.0 6.0 5.0 4.0 3.0 2.0 1.0 225.19620(M+H) + Mass error :0.26ppm C13H25N2O 449.38481(2M+H) + 120 160 200 240 280 320 360 400 440 480 m/z, amu Intensity, counts 10 5 1.1 0.9 0.7 0.5 0.3 403.23316 150 250 350 450 550 650 750 850 950 m/z, amu
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 : 10000 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
N- (0.5ppb) 1 800 2 700 600 500 3 400 300 m/z=237.10-237.11 m/z=242.08-242.09 m/z=275.10-275.11 Intensity, cps 1200 1100 1000 900 800 700 600 500 400 m/z=224.09-224.10 m/z=239.15-139.16 m/z=226.08-226.09 5 6 7 9 200 100 4 300 m/z=116.05-116.06 200 100 m/z=208.13-208.14 8 0 1.0 5.0 9.0 13.0 17.0 Time, min 1.0 5.0 9.0 13.0 17.0 Time, min
- 1.Oxamyl 2.Methiocarbsulfoxide 3.Methiocarbsulfone 4.Aldicarb 5.Bendiocarb 6.Pirimicarb 7.Ethiofencarb 8.Fenobcarb 9.Methiocarb
1 2 Intensity, cps 30000 26000 22000 18000 14000 10000 6000 140000 120000 100000 80000 60000 40000 20000 3 1.0 3.0 5.0 7.0 9.0 11.0 13.0 15.0 17.0 19.0 6 4 5 1.Oxamyl 2.Methiocarbsulfoxide 3.Methiocarbsulfone 4.Aldicarb 5.Bendiocarb 6.Pirimicarb 7.Ethiofencarb 8.Fenobcarb 9.Methiocarb 7 8 9 1.0 3.0 5.0 7.0 9.0 11.0 13.0 15.0 17.0 19.0 Time, min N- (20ppt ppt)
. 200000 200000cps 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 ;2.3 10.1% 10.1%