%0 Journal Article
%T High Performance Liquid Chromatography/Quadrupole Time-of-Flight Mass Spectrometry for the Determination of Brevetoxin PbTx-2 in Shellfish
高效液相色谱/四极杆-飞行时间质谱测定神经性贝毒
%A FANG Xiaoming
%A TANG Yifeng
%A LIU Junping
%A
方晓明
%A 唐毅锋
%A 刘俊平
%J 色谱
%D 2004
%I
%X Brevetoxin PbTx-2 was determined by high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (Q-TOFMS). Extraction from shellfish tissue was achieved with acetone, and purified by solid-phase extraction on a C18 cartridge column. Chromatographic separation was performed on a Zorbax XDB-C18 column(150 mm x 2.1 mm i.d., 3.5 microm) combined with a safeguard column (Symmetry C18, 20 mm i.d. x 3.9 mm, 5 microm) with methanol-water(85: 15, v/v) containing 0.5 mmol/L ammonium acetate as eluent at a flow rate of 0.20 mL/min. The protonated PbTx-2 molecule was selected as a precursor ion scanning for Q-TOFMS in the positive electrospray ionization mode. Average recoveries of PbTx-2 spiked to tissue homogenates through the complete cleanup procedure ranged from 91% to 94%, and relative standard deviations (RSD) ranged from 11% to 12%. The limit of quantification in shellfish tissue was 0.1 microg/g, and the limit of detection based on signal-to-noise ratio of 3 was 0.5 ng. The proposed method was used to confirm PbTx-2 in toxic shellfish. It offers a high degree of specificity because Q-TOFMS with high resolution permits accurate relative molecular mass and fragment ion measurement at no expense of sensitivity.
%K high performance liquid chromatography
%K quadrupole time-of-flight mass spec-trometry
%K neurotoxic shellfish poisoning
%K Brevetoxin PbTx-2
%K shellfish
神经性贝毒
%K 测定
%K 高效液相色谱
%K 四极杆-飞行时间质谱
%K 短裸甲藻毒素
%U http://www.alljournals.cn/get_abstract_url.aspx?pcid=6E709DC38FA1D09A4B578DD0906875B5B44D4D294832BB8E&cid=6579068328FE643F&jid=4D81E042D77AFEC6881D14759692069C&aid=EFA9BB45733AC229&yid=D0E58B75BFD8E51C&vid=BC12EA701C895178&iid=CA4FD0336C81A37A&sid=A04140E723CB732E&eid=EA389574707BDED3&journal_id=1000-8713&journal_name=色谱&referenced_num=3&reference_num=4