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过氧化氢柱前荧光衍生化液相色谱法测定麻痹性贝毒的研究 被引量:8

Determination of Paralytic Shellfish Poisoning Toxins by Liquid Chromatography with Fluorescence Detection Using Pre-column Derivatization with Hydrogen Peroxide Oxidation
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摘要 液相色谱-荧光检测法(LC-FLD)测定贝类样品中石房蛤毒素(STX)和decarbamoylsaxitoxin(dcSTX).样品经30 mmol/L HAc超声提取,C18固相萃取柱净化,2%碱性H2O2荧光衍生,C18色谱柱(4.6 mm×250 mm, 5 μm)分离,以乙腈-0.1 mol/L甲酸铵溶液(5:95,V/V)作流动相,流速1.0 mL/min.结果表明,STX和dcSTX衍生物在7min内获得完全分离.在空白样品中添加标准品使浓度0.01~2.0 μg/g,得到峰面积与浓度呈良好线性,线性相关系数》0.998.添加浓度在0.1、0.8和1.6 μg/g的回收率为87%~97%(n=8);相对标准偏差为8%~13%.方法检出限(S/N=3)分别为STX 1.0 ng/g和dcSTX 0.3 ng/g.另外,采用四极杆-飞行时间质谱(Q-TOF-MS)对STX和dcSTX衍生物进行了结构解析. Saxitoxin (STX) and decarbamoylsaxitoxin (dcSTX) were determined by liquid chromatography with fluorescence detection. A shellfish tissue was extracted with 30 mmol/L HAc under ultrasonication, and cleanup of extract was accomplished by solid-phase extraction with a C18 cartridge. Fluorescence derivatization of STX and dcSTX was used with 2% alkaline H2O2 solution. Chromatographic separation was carried out on a C18 cohmn(4.6 mm × 250 mm,5μm)with elution of acetonitrile-0. 1 mol/L ammonium formate solution (5:95, V/V) at a flow rate of 1.0 mL/min. STX and dcSTX derivatives were completely separated in 7 min. The matrix-matched calibration graphs for STX and dcSTX were prepared by injecting extracted blank spiked with increasing amounts of standard ranging from 0. 01 to 2.0 μg/g, giving an acceptable linearity ( r = 0. 9983 and r = 0. 9989) over the test range. Average recoveries and relative standard deviations, by analyzing samples spiked at a level of 0. 1,0.8 and 1.6μg/g, were 87% -97% and 8% - 13%, respectively. The detection limits ( S/N= 3 ) of STX and dsSTX were 1.0 ng/g and 0. 3 ng/g, respectively. The proposed method is very sensitive, simple, fast and reproducible. In addition, the structures of STX and dcSTX derivatives were elucidated using quadrupole time-of-flight mass spectrometry.
出处 《分析化学》 SCIE EI CAS CSCD 北大核心 2006年第7期933-936,共4页 Chinese Journal of Analytical Chemistry
基金 科技部"十五"攻关专项基金项目(No.2001BA804A20-2-3) 上海市科委基金项目(No.03DZ05045)资助。
关键词 液相色谱 荧光检测 麻痹性贝毒 质谱 Liquid chromatography, fluorescence detection, paralytic shellfish poisoning, mass spectrometry
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