基于N-氨乙基-3-氨丙基甲基二甲氧基硅烷(AEPTS)键合开管柱,研究遗忘性贝类毒素(软骨藻酸,DA)的电色谱分离行为,建立了DA的毛细管开管柱电色谱(OTCEC)快速分析技术.考察并优化了缓冲液类型、缓冲液浓度、p H值、分离电压以及进样时间等参数影响,在最优条件下(20 mmol·L-1Na H2PO4-Na2HPO4缓冲液,p H=4.00,电动进样25 s,进样和分离电压为-18 k V),DA标准溶液在0.12~5.00μg·m L-1范围内线性良好,检测限(S/N=3)为0.03μg·m L-1.应用于扇贝中DA的快速分析,扇贝贝肉提取液无需净化即可直接进样,扇贝中DA线性浓度范围为0.50~10.00μg·m L-1,检测限(S/N=3)为0.25μg·m L-1(相当于贝肉中DA含量1.0μg·g-1),扇贝样品加标回收率为80.5%~83.1%,RSD〈8.5%.
A rapid profile of amnesic shellfish toxin( viz. domoic acid,DA) in shellfish meat has been gained by open- tubular capillary electrochromatography( OTCEC) using an open- tubular column functionalized by 3- [2-( 2- Aminoethylamino- ethylamino]propyl trimethoxysilane( AEPTS). The chromatographic behavior of DA in OTCEC was studied,and the effects of several analytical parameters including the composition,p H value and concentration of the buffer solution,separation voltage,and the injection value were investigated and optimized. Under the optimal conditions( Na H2PO4- Na2HPO4 bufffer,20 mmol·L- 1,p H 4. 00,injection voltage- 18 k V,separation voltage- 18 k V,injection time 25 s),a linear relationship between the DA concentration and CE peak intensity could be obtained in the range of 0. 12 to 5. 00 μg·m L- 1with a detection limit( S / N =3) of 0. 03 μg·m L- 1. Applied to shellfish foods,the extraction samples of scallop meats could be directly detected without any purification treatment. The calibration curve of real extraction samples of scallop tissue was obtained from 0. 50 to 10. 00 μg·m L- 1,and the detection limit( S /N = 3) of 0. 25μg·m L- 1( equal to the content of DA at 1. 0 μg·g- 1in total tissues). Satisfactory recoveries of fortified samples ranged from 80. 5% to 83. 1% were obtained with the RSD less than 8. 5%.