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

被引:153
作者
Crescenzi, C
Bayoudh, S
Cormack, PAG
Klein, T
Ensing, K
机构
[1] Univ Groningen, Ctr Pharm, Dept Analyt Chem & Toxicol, Groningen, Netherlands
[2] Univ Strathclyde, Dept Pure & Appl Chem, Glasgow, Lanark, Scotland
关键词
D O I
10.1021/ac0014360
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
Matrix solid-phase dispersion(MSPD) is a new sample pretreatment for solid samples. This technique greatly simplifies sample pretreatment but, nonetheless, the extracts often still require an extra cleanup step that is both laborious and time-consuming. The potential;of combining MSPD with molecularly 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 cartridge. Subsequently, clenbuterol was eluted from the MSPD cartridge onto the MISPE cartridge using acetonitrile containing 1% acetic acid.:The ability of the molecularly imprinted polymer to selectively adsorb analyte in acetonitrile was exploited for re-extracting clenbuterol directly from this acetonitrile extract via the double cartridge tandem system. The analyte was eluted from the MISPE cartridge using acidified methanol, A clear eluate was obtained, 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 cartridges showed excellent stability. The complete extraction procedure was rapid,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.
引用
收藏
页码:2171 / 2177
页数:7
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