SPE of Tetracyclines from Honey Using Gemini 5u
LC Conditions
Column
Gemini 5 µm C18 110 Å, LC Column 150 x 3 mm, Ea
Brand
Gemini
Part No
00F-4435-Y0
Phase Name
C18
Elution Type
Isocratic
Mobile Phase
A: 10 mm Oxalic acid
B: Acetonitrile
Gradient Profile
Step No.
Time(min)
%A
%B
1
0
80
20
Flow Rate
0.80 mL/min
Temperature
22°C
Detection
UV-Vis Abs.-Variable Wave.(UV) @ (22°C)
Detection Info
Sample Notes
SecurityGuard™ Guard Cartridge System extends column lifetime. - SecurityGuard Cartridges, Gemini C18 4 x 2.0mm, 10/Pk Part No.: AJ0-7596 - Holder Part No.: KJ0-4282
Sample Preparation Details
Description
Strata-X-CW 33 µm Polymeric Weak Cation, 60 mg / 3 mL, Tubes, 50/Pk
Part No
8B-S035-UBJ
Pretreatment Note
Elution of 2 mL (2% Formic Acid in Methanol) is recommended to do in 2 aliquots
Condition 1
2 mL MeOH at 1 mL/min
Condition 2
2 mL Water at 1 mL/min
Sample Pretreatment
The SPE extract looks so clean that conc. down to 50 ng/mL (100ng on column injection by conentrating the SPE extract) can be achievable without much background noise.
Load
Load 4.00 mL Sample diluted in NaOAc (100mM) pH 5.0
Wash 1
4 mL Water at 1 mL/min
Wash 2
4 mL Methanol at 1 mL/min
Wash 3
2 mL 2% Formic Acid in Methanol at 1 mL/min
Dry
2 min at 10 of Hg
Elution 1
2 mL 2% Formic Acid in Methanol at 1 mL/min
Evaporation
Evaporate to dryness
Reconstitute
100 µL 10mM oxalic acid (pH2)/ACN=80/20
Order Items Used in This Application
- 1. Oxytetracycline
- 2. Tetracycline
- 3. Chlortetracycline
-OEChem-05081000432D<br><br> 57 60 0 1 0 0 0 0 0999 V2000<br> 6.9338 1.9246 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.0678 -1.5754 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 9.1837 1.8310 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.9338 -2.0754 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 8.6822 -2.1100 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.6839 -1.9818 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.4037 0.9488 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 10.5194 -2.1530 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.4075 -2.0995 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.1854 1.9592 0.0000 N 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.5357 -0.6029 0.0000 N 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.0678 0.4246 0.0000 C 0 0 2 0 0 0 0 0 0 0 0 0<br> 7.7998 0.4246 0.0000 C 0 0 2 0 0 0 0 0 0 0 0 0<br> 6.9338 0.9246 0.0000 C 0 0 2 0 0 0 0 0 0 0 0 0<br> 6.0678 -0.5754 0.0000 C 0 0 1 0 0 0 0 0 0 0 0 0<br> 5.1738 0.9593 0.0000 C 0 0 1 0 0 0 0 0 0 0 0 0<br> 8.6938 0.9593 0.0000 C 0 0 1 0 0 0 0 0 0 0 0 0<br> 7.7998 -0.5754 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.9338 -1.0754 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.1738 -1.1100 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 9.5998 0.4455 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.2678 0.4455 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 8.6938 -1.1100 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 8.1838 1.8195 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 9.5998 -0.5962 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.2678 -0.5962 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 10.5310 1.0024 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.3252 2.4692 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.0572 2.4492 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 10.5310 -1.1531 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.4037 -1.0995 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 11.4748 0.4671 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 11.4748 -0.6179 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.0743 1.2746 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 7.7933 1.2746 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.3969 1.2346 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.7149 1.2620 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 8.7171 2.1357 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 7.8676 2.3528 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 7.6505 1.5033 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 7.4707 2.2346 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.7578 -2.1123 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 8.8675 2.3644 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 10.5238 1.6223 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.6414 3.0025 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.7919 2.7854 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.0090 1.9359 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.3609 1.9087 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 6.5976 2.7530 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 5.7534 2.9897 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 9.2155 -2.4261 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 12.0105 0.7792 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 12.0105 -0.9299 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.0000 -0.9149 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.5334 0.0171 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 11.0528 -2.4692 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.8718 -2.4116 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 14 1 1 1 0 0 0<br> 1 41 1 0 0 0 0<br> 15 2 1 1 0 0 0<br> 2 42 1 0 0 0 0<br> 17 3 1 6 0 0 0<br> 3 43 1 0 0 0 0<br> 4 19 2 0 0 0 0<br> 5 23 1 0 0 0 0<br> 5 51 1 0 0 0 0<br> 6 20 2 0 0 0 0<br> 7 22 2 0 0 0 0<br> 8 30 1 0 0 0 0<br> 8 56 1 0 0 0 0<br> 9 31 1 0 0 0 0<br> 9 57 1 0 0 0 0<br> 16 10 1 1 0 0 0<br> 10 28 1 0 0 0 0<br> 10 29 1 0 0 0 0<br> 11 31 1 0 0 0 0<br> 11 54 1 0 0 0 0<br> 11 55 1 0 0 0 0<br> 12 14 1 0 0 0 0<br> 12 15 1 0 0 0 0<br> 12 16 1 0 0 0 0<br> 12 34 1 1 0 0 0<br> 13 14 1 0 0 0 0<br> 13 17 1 0 0 0 0<br> 13 18 1 0 0 0 0<br> 13 35 1 1 0 0 0<br> 14 36 1 0 0 0 0<br> 15 19 1 0 0 0 0<br> 15 20 1 0 0 0 0<br> 16 22 1 0 0 0 0<br> 16 37 1 0 0 0 0<br> 17 21 1 0 0 0 0<br> 17 24 1 0 0 0 0<br> 18 19 1 0 0 0 0<br> 18 23 2 0 0 0 0<br> 20 26 1 0 0 0 0<br> 21 25 2 0 0 0 0<br> 21 27 1 0 0 0 0<br> 22 26 1 0 0 0 0<br> 23 25 1 0 0 0 0<br> 24 38 1 0 0 0 0<br> 24 39 1 0 0 0 0<br> 24 40 1 0 0 0 0<br> 25 30 1 0 0 0 0<br> 26 31 2 0 0 0 0<br> 27 32 2 0 0 0 0<br> 27 44 1 0 0 0 0<br> 28 45 1 0 0 0 0<br> 28 46 1 0 0 0 0<br> 28 47 1 0 0 0 0<br> 29 48 1 0 0 0 0<br> 29 49 1 0 0 0 0<br> 29 50 1 0 0 0 0<br> 30 33 2 0 0 0 0<br> 32 33 1 0 0 0 0<br> 32 52 1 0 0 0 0<br> 33 53 1 0 0 0 0<br>M END
Compound Name
Oxytetracycline
CID
5280972
Molecular Formula
C22H24N2O9
Molecular Weight
460
No. Hydrogen Bond Acceptors
11
No. Hydrogen Bond Donors
7
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