Determination of clenbuterol in bovine liver by combining matrix solid phase dispersion and molecularly imprinted solid phase extraction followed by liquid chromatography/electrospray ion trap multiple stage mass spectrometry
C. Crescenzi et al., Determination of clenbuterol in bovine liver by combining matrix solid phase dispersion and molecularly imprinted solid phase extraction followed by liquid chromatography/electrospray ion trap multiple stage mass spectrometry, ANALYT CHEM, 73(10), 2001, pp. 2171-2177
Matrix solid-phase dispersion(MSPD) is a new sample pretreatment for solid
samples. This technique greatly simplifies sample pretreatment but, nonethe
less, the extracts often still require an extra cleanup step that is both l
aborious and time-consuming. The potential;of combining MSPD with molecular
ly imprinted solid-phase extraction (MISPE) was investigated in this study.
Liver samples were ground in a mortar with Cls sorbent and the homogenized
mixture packed into an SPE cartridge and placed on top of a MISPE cartridg
e. Subsequently, clenbuterol was eluted from the MSPD cartridge onto the MI
SPE cartridge using acetonitrile containing 1% acetic acid.:The ability of
the molecularly imprinted polymer to selectively adsorb analyte in acetonit
rile was exploited for re-extracting clenbuterol directly from this acetoni
trile extract via the double cartridge tandem system. The analyte was elute
d from the MISPE cartridge using acidified methanol, A clear eluate was obt
ained, which was subsequently evaporated, redissolved, and analyzed by HPLC
electrochemical detection (ECD) or ion trap mass spectrometry (LC/IT-MS).
The MISPE cartridge used in this study was imprinted using bromoclenbuterol
, a structural analogue of clenbuterol, as the template. These MISPE cartri
dges showed excellent stability. The complete extraction procedure was rapi
d,and recoveries exceeded 90% for the target analyte. The method detection
limit for the LC/IT-MS procedure was < 0.1 mug/kg. This method, therefore,
satisfies the stringent requirements of European Union regulation EEC 2377/
90.