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首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >Application of solid phase microextraction in the determination of paralytic shellfish poisoning toxins
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Application of solid phase microextraction in the determination of paralytic shellfish poisoning toxins

机译：固相微萃取在麻痹性贝类中毒毒素测定中的应用

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摘要

A SPME-HPLC-post-column fluorescent derivatization method for the direct determination of saxitoxin (STX),the most potent paralytic shellfish poisoning (PSP) toxin,in water has been developed.Commercially available SPME devices with 50 mum Carbowax templated resin (CW/TPR) coating was found to be able to pre-concentrate STX from aqueous media.A special pre-conditioning treatment of soaking the SPME coating in 0.1 M NaOH solution significantly improved the extraction efficiency.The optimal pH for the SPME process is 8.1 and the equilibration time is 40 min.The partition coefficient,K,of the distribution of STX between the SPME coating and the aqueous media was measured to be 2.99 +- 0.04 x 10~3.Extracted toxin on the SPME stationary phase was difficult to be desorbed by the HPLC mobile phase under dynamic desorption mode.A static ion-pairing desorption technique using a desorption solvent mixture of 20 mM sodium 1 -heptanesulfonate in 30% aqueous acetonitrile acidified with 50 mM sulfuric acid was developed to overcome this problem.The method detection limit and repeatability achieved by this SPME-HPLC method were 0.11 ng ml~(-1) and 3.7%,respectively,with a sample volume of just 5 ml of water.This analytical method is adequate for the monitoring of the PSP toxin in fresh/drinking waters.However,serious interference was observed when this technique was applied to saline water samples.This is probably due to competition of sodium ions with the cationic STX for absorption into the SPME stationary phase.
机译：开发了一种SPME-HPLC后柱荧光衍生化方法，可直接测定水中最有效的麻痹性贝类中毒（PSP）毒素-毒素（50毫克Carbowax模板树脂（CW）的市售SPME设备。 / TPR）涂层能够从水性介质中预浓缩STX。特殊的预处理处理将SPME涂层浸泡在0.1 M NaOH溶液中可显着提高萃取效率.SPME工艺的最佳pH为8.1和平衡时间为40分钟。测得SPTX涂层与水性介质之间的STX分配的分配系数K为2.99 +-0.04 x 10〜3。很难在SPME固定相上提取毒素在动态解吸模式下由HPLC流动相解吸静态离子对解吸技术，使用20 mM 1-庚烷磺酸钠在30％乙腈水溶液中的解吸溶剂混合物（用50 mM硫酸化）为了克服这个问题而开发了硫酸。该SPME-HPLC方法的检测限和重现性分别为0.11 ng ml〜（-1）和3.7％，样品量仅为5 ml水。该方法足以监测淡水/饮用水中的PSP毒素。但是，此技术应用于盐水样品时会观察到严重干扰，这可能是由于钠离子与阳离子STX竞争吸收到SPME中固定相。

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