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Penicillins in Meat by LC/MS/MS

Sample Preparation Details

Part No:8B-S001-FBJ
Solid Phase Extraction (SPE) procedure:Note: The solvent volumes shown below are for a 200 mg bed mass. The solvent volumes will need to be adjusted for a smaller or larger bed mass.
Load:Homogenize the sample using an electric mincer. Measure 4 g of the homogenized sample into an 85 mL centrifuge tube. Add 20 m L of acetonitrile/water (10:1). Mix for 1 min using an Ultra-Turrax mixer at a velocity setting of 2. Agitate further for 5 min using an orbital mixer at a velocity setting of 100. Centrifuge at 4400 rpm, 10 C for 15 min. Filter 5 mL of the top liquid layer through a 45 um Phenex filter. Mix 1.97 g of KH2PO4 and 2.8 mL KOH 5M in 200 mL of water and filter this mixture. Mix 0.25 mL of the filtreate with 4.75 mL of McIlvaine buffer (pH 7.6).
Final Prep and Analysis: The equilibration time at conditon 0 was 4 minutes before each injection. Inject: 50 µL on HPLC / Tandem Mass Spec (MS-MS) @ -4500 V (600 °C)

Analytes:

Name Spiked
Conc.
Log P pKa % Rec %RSC (n=0)
1 Amoxicillin
2 Ampicillin
3 Penicillin G
4 Penicillin V
5 Oxacillin
6 Cloxacillin
7 Nafcillin
8 Dicloxacillin

Application Detail (App ID: 20028)

Part No:00F-4439-E0
Dimensions:150 x 4.6 mm ID
Elution Type:Gradient
Elution A:0.1% Ammonia in water
Elution B:95% Acetronitrile, 5% water and 0.1% ammonia
Gradient Profile:
Step No. Time (min) Pct A Pct B
1 0 98 2
2 2 98 2
3 2.42 90 10
4 6 50 50
5 6.1 0 100
6 6.6 0 100
7 6.8 98 2
8 8 98 2

Flow Rate:0.8 mL/min
Col. Temp: 40 °C
Detection: Tandem Mass Spec (MS-MS) @ -4500 V (600°C)
Detector Info: 3200 QTRAP
Note:This separation uses IMethod Kit Part Number KH0-9047

SecurityGuard™ Guard Cartridge System extends column lifetime.
- SecurityGuard Cartridges, Gemini C18 4 x 3.0mm ID, 10/Pk Part No.: AJ0-7597
- Holder Part No.: KJ0-4282

Analyte Details

Analyte Detail not available

1
Amoxicillin
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2
Ampicillin
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3
Penicillin G
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4
Penicillin V
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5
Oxacillin
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6
Cloxacillin
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7
Nafcillin
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8
Dicloxacillin
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