Extraction of Timolol from Serum using Strata-X-C 10 mg Plate & Kinetex 2.6u Biphenyl 50x2.1 Column

Extraction of Timolol from Serum using Strata-X-C 10 mg Plate & Kinetex 2.6u Biphenyl 50x2.1 Column
LC Conditions
Column

Kinetex 2.6 µm Biphenyl 100 Å, LC Column 50 x 2.1 mm, Ea

Brand

Kinetex

Part No

00B-4622-AN

Phase Name

Biphenyl

Elution Type

Gradient

Mobile Phase

A: 0.1% formic acid in water

B: 0.1% formic acid in acetonitrile

Gradient Profile

Step No.

Time(min)

%A

%B

1

0

95

5

2

0.5

95

5

3

3

5

95

4

3.5

5

95

5

3.51

95

5

6

5.5

95

5

Flow Rate

0.50 mL/min

Temperature

25°C

Detection

Tandem Mass Spec (MS-MS) @ (22°C)

Detection Info
Sample Notes

Strata X-C 10 mg Plate Protocol Condition 500 µL methanol Equilibrate 500uL water Load 750 µL diluted serum (375 µL plasma diluted 1:1 with 4% phosphoric acid in water) Wash1 500 µL 2% formic acid in water Wash 2 500 µL methanol Elute 375 µL(3x125 µL) 5% ammonium hydroxide in acetonitrile:methanol(60:40) Inject 1 µL Note: Spiked conc. of analyte was 1 ng/mL serum

Sample Preparation Details
Description

Strata X-C 33 µm Polymeric Strong Cation, 10 mg / well, 96-Well Plates, 2/Pk

Part No

8E-S029-AGB

Pretreatment Note

No dry down step was performed. 1µL of final eluent was injected.

Condition 1

0.5 mL Methanol

Condition 2

0.5 mL Water

Load

Load 375.00 µL Sample diluted in 375 µL 4% Phosphoric acid in water

Wash 1

0.5 mL 2% Formic acid in water

Wash 2

0.5 mL Methanol

Elution 1

0.125 mL 5% Ammonium hydroxide in Acetonitrile/Methanol (60:40)

Elution 2

0.125 mL 5% Ammonium hydroxide in Acetonitrile/Methanol (60:40)

Elution 3

0.125 mL 5% Ammonium hydroxide in Acetonitrile/Methanol (60:40)

Evaporation

Evaporate to dryness

Order Items Used in This Application

Strata X-C 33 µm Polymeric Strong Cation, 10 mg / well, 96-Well Plates, 2/Pk
8E-S029-AGB

Strata X-C 33 µm Polymeric Strong Cation, 10 mg / well, 96-Well Plates, 2/Pk

View Product

Kinetex 2.6 µm Biphenyl 100 Å, LC Column 50 x 2.1 mm, Ea
00B-4622-AN

Kinetex 2.6 µm Biphenyl 100 Å, LC Column 50 x 2.1 mm, Ea

View Product

  • 1. Timolol
-OEChem-05081000432D<br><br> 45 46  0     1  0  0  0  0  0999 V2000<br>    2.3660   -1.8332    0.0000 S   0  0  0  0  0  0  0  0  0  0  0  0<br>    2.8660    2.7056    0.0000 O   0  0  0  0  0  0  0  0  0  0  0  0<br>    4.6261   -0.5731    0.0000 O   0  0  0  0  0  0  0  0  0  0  0  0<br>    6.5282    0.0449    0.0000 O   0  0  0  0  0  0  0  0  0  0  0  0<br>    8.0145   -1.2934    0.0000 N   0  0  0  0  0  0  0  0  0  0  0  0<br>    2.8660    0.7056    0.0000 N   0  0  0  0  0  0  0  0  0  0  0  0<br>    2.0570   -0.8822    0.0000 N   0  0  0  0  0  0  0  0  0  0  0  0<br>    3.3660   -1.8332    0.0000 N   0  0  0  0  0  0  0  0  0  0  0  0<br>    8.7576   -1.9625    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    7.0634   -1.6024    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    6.3203   -0.9332    0.0000 C   0  0  1  0  0  0  0  0  0  0  0  0<br>    3.7320    1.2056    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    2.0000    1.2056    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    9.5008   -2.6316    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    9.4268   -1.2194    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    8.0885   -2.7056    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    3.7320    2.2056    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    2.0000    2.2056    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    5.3692   -1.2423    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    2.8660   -0.2944    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    3.6750   -0.8822    0.0000 C   0  0  0  0  0  0  0  0  0  0  0  0<br>    8.1434   -0.6869    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    6.5749   -1.9841    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    7.3545   -2.1498    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    5.8595   -0.5184    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    3.9441    0.6230    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    4.3426    1.3133    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    1.3894    1.3133    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    1.7880    0.6230    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    9.0859   -3.0924    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    9.9615   -3.0465    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    9.9156   -2.1709    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    9.8875   -1.6342    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    9.8416   -0.7586    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    8.9660   -0.8045    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    7.6278   -2.2908    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    7.6737   -3.1664    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    8.5493   -3.1205    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    4.3426    2.0980    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    3.9441    2.7882    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    1.7880    2.7882    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    1.3894    2.0980    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    4.8807   -1.6240    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    5.6603   -1.7897    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>    7.1179    0.2365    0.0000 H   0  0  0  0  0  0  0  0  0  0  0  0<br>  1  7  1  0  0  0  0<br>  1  8  1  0  0  0  0<br>  2 17  1  0  0  0  0<br>  2 18  1  0  0  0  0<br>  3 19  1  0  0  0  0<br>  3 21  1  0  0  0  0<br> 11  4  1  1  0  0  0<br>  4 45  1  0  0  0  0<br>  5  9  1  0  0  0  0<br>  5 10  1  0  0  0  0<br>  5 22  1  0  0  0  0<br>  6 12  1  0  0  0  0<br>  6 13  1  0  0  0  0<br>  6 20  1  0  0  0  0<br>  7 20  2  0  0  0  0<br>  8 21  2  0  0  0  0<br>  9 14  1  0  0  0  0<br>  9 15  1  0  0  0  0<br>  9 16  1  0  0  0  0<br> 10 11  1  0  0  0  0<br> 10 23  1  0  0  0  0<br> 10 24  1  0  0  0  0<br> 11 19  1  0  0  0  0<br> 11 25  1  0  0  0  0<br> 12 17  1  0  0  0  0<br> 12 26  1  0  0  0  0<br> 12 27  1  0  0  0  0<br> 13 18  1  0  0  0  0<br> 13 28  1  0  0  0  0<br> 13 29  1  0  0  0  0<br> 14 30  1  0  0  0  0<br> 14 31  1  0  0  0  0<br> 14 32  1  0  0  0  0<br> 15 33  1  0  0  0  0<br> 15 34  1  0  0  0  0<br> 15 35  1  0  0  0  0<br> 16 36  1  0  0  0  0<br> 16 37  1  0  0  0  0<br> 16 38  1  0  0  0  0<br> 17 39  1  0  0  0  0<br> 17 40  1  0  0  0  0<br> 18 41  1  0  0  0  0<br> 18 42  1  0  0  0  0<br> 19 43  1  0  0  0  0<br> 19 44  1  0  0  0  0<br> 20 21  1  0  0  0  0<br>M  END
Compound Name

Timolol

CID

33624

Molecular Formula

C13H24N4O3S

Molecular Weight

316

No. Hydrogen Bond Acceptors

7

No. Hydrogen Bond Donors

2

Similar Applications

Reversed Phase

Beta-blockers using Luna Omega 1.6u PS C18 50x2.1mm

Luna Omega 1.6µm PS C18 100Å, LC Column 50 x 2.1 mm, EA

23727

Reversed Phase

Beta-blockers using Luna Omega Polar C18 50x2.1mm

Luna Omega 1.6µm Polar C18 100Å, LC Column 50 x 2.1 mm, EA

23611