PMID- 19402673
OWN - NLM
STAT- MEDLINE
DCOM- 20090805
LR  - 20191210
IS  - 1520-6882 (Electronic)
IS  - 0003-2700 (Linking)
VI  - 81
IP  - 11
DP  - 2009 Jun 1
TI  - Fully automated analysis of beta-lactams in bovine milk by online solid phase 
      extraction-liquid chromatography-electrospray-tandem mass spectrometry.
PG  - 4285-95
LID - 10.1021/ac9001386 [doi]
AB  - A fully automated method for the detection of beta-lactam antibiotics, including 
      six penicillins (amoxicillin, ampicillin, cloxacillin, dicloxacillin, oxacillin, 
      and penicillin G) and four cephalosporins (cefazolin, ceftiofur, cefoperazone, 
      and cefalexin) in bovine milk samples has been developed. The outlined method is 
      based on online solid-phase extraction-liquid chromatography/electrospray-tandem 
      mass spectrometry (SPE-LC/ESI-MS-MS). Target compounds were concentrated from 500 
      microL of centrifuged milk samples using an online SPE procedure with C18 HD 
      cartridges. Target analytes were eluted with a gradient mobile phase (water + 
      0.1% formic acid/methanol + 0.1% formic acid) at a flow rate of 0.7 mL/min. 
      Chromatographic separation was achieved within 10 min using a C-12 reversed phase 
      analytical column. For unequivocal identification and confirmation, two multiple 
      reaction monitoring (MRM) transitions were acquired for each analyte in the 
      positive electrospray ionization mode (ESI(+)). Method limits of detection (LODs) 
      in milk were well below the maximum residue limits (MRLs) set by the European 
      Union for all compounds. Limits of quantification in milk were between 0.09 ng/mL 
      and 1.44 ng/mL. The developed method was validated according to EU's 
      requirements, and accuracy results ranged from 80 to 116%. Finally, the method 
      was applied to the analysis of twenty real samples previously screened by the 
      inhibition of microbial growth test Eclipse 100. This new developed method offers 
      high sensitivity and accuracy of results, minimum sample pre-treatment, and uses 
      for the first time an automated online SPE offering a high throughput analysis. 
      Because of all these characteristics, the proposed method is applicable and could 
      be deemed necessary within the field of food control and safety.
FAU - Kantiani, Lina
AU  - Kantiani L
AD  - Department of Environmental Chemistry, IDAEA-CSIC, c/Jordi Girona 18-26, 08034, 
      Barcelona, Spain.
FAU - Farre, Marinella
AU  - Farre M
FAU - Sibum, Martin
AU  - Sibum M
FAU - Postigo, Cristina
AU  - Postigo C
FAU - Lopez de Alda, Miren
AU  - Lopez de Alda M
FAU - Barcelo, Damia
AU  - Barcelo D
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PT  - Validation Study
PL  - United States
TA  - Anal Chem
JT  - Analytical chemistry
JID - 0370536
RN  - 0 (Anti-Bacterial Agents)
RN  - 0 (beta-Lactams)
SB  - IM
MH  - Animals
MH  - Anti-Bacterial Agents/*analysis
MH  - Cattle
MH  - Chromatography, Liquid/*methods
MH  - Equipment Design
MH  - Milk/*chemistry
MH  - Sensitivity and Specificity
MH  - Solid Phase Extraction/instrumentation/*methods
MH  - Spectrometry, Mass, Electrospray Ionization/methods
MH  - Tandem Mass Spectrometry/*methods
MH  - beta-Lactams/*analysis
EDAT- 2009/05/01 09:00
MHDA- 2009/08/06 09:00
CRDT- 2009/05/01 09:00
PHST- 2009/05/01 09:00 [entrez]
PHST- 2009/05/01 09:00 [pubmed]
PHST- 2009/08/06 09:00 [medline]
AID - 10.1021/ac9001386 [doi]
PST - ppublish
SO  - Anal Chem. 2009 Jun 1;81(11):4285-95. doi: 10.1021/ac9001386.