Analysis of Phenylbutazone on Kinetex 2.6u XB-C18 50x2.1 by LC-MS-MS API 4000
LC Conditions
Column
Kinetex 2.6 µm XB-C18 100 Å, LC Column 50 x 2.1 mm, Ea
Brand
Kinetex
Part No
00B-4496-AN
Phase Name
XB-C18
Elution Type
Gradient
Mobile Phase
A: 0.1% Formic Acid in DI Water
B: 0.1% Formic Acid in Methanol
Gradient Profile
Step No.
Time(min)
%A
%B
1
0
50
50
2
0.5
50
50
3
2
5
95
4
3.5
5
95
5
3.51
50
50
6
5
50
50
Flow Rate
0.45 mL/min
Temperature
45°C
Detection
Mass Spectrometer (MS) @ (0°C)
Detection Info
Sample Notes
Mass spec conditions: API 4000, ESI TurboIon Spray, + Ionization; CAD: 6.00 CUR: 20.00 GS1: 50.00 GS2: 50.00 IS: 5500.00 TEM: 600.00 ihe: ON DP 50.00 EP 10.00
Sample Preparation Details
Pretreatment Note
Sample Pre-Treatment (before SPE): Protein precipitation: To 0.5 mL whole blood (spiked with analytes) add 1.0 mL cold AcCN: MeOH 85:15, vortex 1-2 mins (using a maximix II, from Barnstead) with the maximum force possible, followed by centrifugation at 10,000 rpm, for 10 mins
Load
Load 1.50 mL Sample diluted in 3 mL of 1% Formic acid in water
Wash 1
2 mL ACN: Water (15:85)
Dry
5 mins at 10 of Hg
Elution 1
2 mL Ethyl acetate: Isopropanol 85:15
Evaporation
Evaporate to dryness
Reconstitute
500 µL Initial mobile phase (A/B=50/50)
Order Items Used in This Application
- 1. Phenylbutazone
- 2. Phenylbutazone-d10
- 3. impurity
-OEChem-06211003152D<br><br> 43 45 0 0 0 0 0 0 0999 V2000<br> 2.0000 -0.7132 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.8479 1.3559 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.7601 -0.9920 0.0000 N 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.5691 -0.4042 0.0000 N 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.2601 0.5469 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.6723 1.3559 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.9511 -0.4042 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.2601 0.5469 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.0790 2.2694 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.4912 3.0784 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.7601 -1.9920 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.5202 -0.7132 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.8980 3.9920 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.6261 -2.4920 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.2633 -0.0441 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.8940 -2.4920 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.7281 -1.6914 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.6261 -3.4920 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 7.2144 -0.3531 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.8940 -3.4920 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.6791 -2.0004 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.7601 -3.9920 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 7.4223 -1.3312 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.5416 1.0993 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.1583 1.7026 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.2416 0.9099 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.5930 1.9227 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.5097 2.7154 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 1.9772 3.4251 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.0606 2.6324 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.4644 3.7398 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.1502 4.5584 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.3316 4.2442 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.1630 -2.1820 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.1344 0.5624 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.3571 -2.1820 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.2673 -2.1062 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.1630 -3.8020 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 7.6751 0.0618 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.3571 -3.8020 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.8080 -2.6068 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.7601 -4.6120 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 8.0119 -1.5228 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 1 7 2 0 0 0 0<br> 2 8 2 0 0 0 0<br> 3 4 1 0 0 0 0<br> 3 7 1 0 0 0 0<br> 3 11 1 0 0 0 0<br> 4 8 1 0 0 0 0<br> 4 12 1 0 0 0 0<br> 5 6 1 0 0 0 0<br> 5 7 1 0 0 0 0<br> 5 8 1 0 0 0 0<br> 5 24 1 0 0 0 0<br> 6 9 1 0 0 0 0<br> 6 25 1 0 0 0 0<br> 6 26 1 0 0 0 0<br> 9 10 1 0 0 0 0<br> 9 27 1 0 0 0 0<br> 9 28 1 0 0 0 0<br> 10 13 1 0 0 0 0<br> 10 29 1 0 0 0 0<br> 10 30 1 0 0 0 0<br> 11 14 2 0 0 0 0<br> 11 16 1 0 0 0 0<br> 12 15 2 0 0 0 0<br> 12 17 1 0 0 0 0<br> 13 31 1 0 0 0 0<br> 13 32 1 0 0 0 0<br> 13 33 1 0 0 0 0<br> 14 18 1 0 0 0 0<br> 14 34 1 0 0 0 0<br> 15 19 1 0 0 0 0<br> 15 35 1 0 0 0 0<br> 16 20 2 0 0 0 0<br> 16 36 1 0 0 0 0<br> 17 21 2 0 0 0 0<br> 17 37 1 0 0 0 0<br> 18 22 2 0 0 0 0<br> 18 38 1 0 0 0 0<br> 19 23 2 0 0 0 0<br> 19 39 1 0 0 0 0<br> 20 22 1 0 0 0 0<br> 20 40 1 0 0 0 0<br> 21 23 1 0 0 0 0<br> 21 41 1 0 0 0 0<br> 22 42 1 0 0 0 0<br> 23 43 1 0 0 0 0<br>M END
Compound Name
Phenylbutazone
CID
4781
Molecular Formula
C19H20N2O2
Molecular Weight
308
No. Hydrogen Bond Acceptors
2
Similar Applications
Reversed Phase
Analysis of Phenylbutazone on Kinetex 2.6u XB-C18 50x2.1 by LC-MS-MS API 4000
Kinetex 2.6 µm XB-C18 100 Å, LC Column 50 x 2.1 mm, Ea
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