PMID- 16008059
OWN - NLM
STAT- MEDLINE
DCOM- 20050829
LR  - 20191210
IS  - 0021-9673 (Print)
IS  - 0021-9673 (Linking)
VI  - 1080
IP  - 2
DP  - 2005 Jul 8
TI  - Determination of microcystins in fish by solvent extraction and liquid 
      chromatography.
PG  - 199-203
AB  - A liquid chromatography electrospray mass spectrometry (LC/ESI/MS) method has 
      been developed to identify and quantify microcystins in fish liver and intestine. 
      Microcystins (MCs) were extracted from 500 mg sample with methanol-water (85:25, 
      v/v) and the extracts concentrated to 250 microl. The parameters were optimized 
      by a full factorial 2(3) design. Neither laborious pre-treatment nor clean up 
      were necessary. MCs were separated using conventional C18 column and an 
      acetonitrile-acidified water (pH 3) gradient. Negative samples (without MCs) were 
      discriminated by liquid chromatography diode array detection (LC/DAD). The limits 
      of detection (LOD) and the limits of quantification (LOQ) resulted equal for 
      MC-RR, MC-YR, and MC-LR and were 0.1 and 0.5 microg g(-1), respectively. MCs 
      recoveries at three levels in spiked samples (0.5-3.0 microg g(-1)) were > 92%, 
      with relative standards deviations (RSDs) < 16% for liver samples and > 68% with 
      RSDs < 18% for intestine samples. The proposed method was applied to determine 
      MC-LR in exposed fish to evaluate the bioaccumulation risk. The results showed 
      the transference of MC-LR from cyanobacterial cells to fish tissues.
FAU - Moreno, Isabel Maria
AU  - Moreno IM
AD  - Area de Toxicologia, Facultad de Farmacia, Universidad de Sevilla, 41012 Sevilla, 
      Spain.
FAU - Molina, Rafael
AU  - Molina R
FAU - Jos, Angeles
AU  - Jos A
FAU - Pico, Yolanda
AU  - Pico Y
FAU - Camean, Ana Maria
AU  - Camean AM
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PT  - Validation Study
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Bacterial Toxins)
RN  - 0 (Marine Toxins)
RN  - 0 (Microcystins)
RN  - 0 (Peptides, Cyclic)
RN  - 77238-39-2 (microcystin)
RN  - EQ8332842Y (cyanoginosin LR)
SB  - IM
MH  - Animals
MH  - Bacterial Toxins/*isolation & purification
MH  - Chemical Fractionation/methods
MH  - Chromatography, Liquid/*methods
MH  - Cyanobacteria/chemistry
MH  - Intestines/chemistry
MH  - Liver/chemistry
MH  - Male
MH  - Marine Toxins/*isolation & purification
MH  - Microcystins
MH  - Peptides, Cyclic/*isolation & purification
MH  - Spectrometry, Mass, Electrospray Ionization/methods
MH  - Tilapia
EDAT- 2005/07/13 09:00
MHDA- 2005/08/30 09:00
CRDT- 2005/07/13 09:00
PHST- 2005/07/13 09:00 [pubmed]
PHST- 2005/08/30 09:00 [medline]
PHST- 2005/07/13 09:00 [entrez]
AID - S0021-9673(05)01022-8 [pii]
AID - 10.1016/j.chroma.2005.05.029 [doi]
PST - ppublish
SO  - J Chromatogr A. 2005 Jul 8;1080(2):199-203. doi: 10.1016/j.chroma.2005.05.029.