Hatfield C L, Wekell J C, Gauglitz E J, Barnett H J
U.S. Department of Commerce, National Oceanic and Atmospheric Administration, Northwest Fisheries Science Center, Seattle, Washington 98112.
Nat Toxins. 1994;2(4):206-11. doi: 10.1002/nt.2620020409.
Domoic acid (DA) was first reported in mussels from Prince Edward Island, Canada, in 1987. It reappeared in anchovies and pelicans from Monterey Bay, California, in 1991. Later that year, domoic acid was found in razor clams and Dungeness crabs along the Washington and Oregon coasts. Since the initial outbreak, a variety of analytical methods for the detection of this neurotoxin have been developed. Here, we describe a modification to the solid phase extraction (SPE) clean-up step in Quilliam's HPLC-UV method (1991: NRCC No. 33001). The standard 10% acetonitrile (MeCN) wash and 0.5M ammonium citrate buffer (ACB) in 10% MeCN (pH = 4.5) eluting solution have been replaced with a 0.1M sodium chloride (NaCl) in 10% MeCN wash and a 0.5M NaCl in 10% MeCN eluting solution. This modification allows the analysis to work equally well on both clam and crab viscera and meat. Chromatograms of visceral samples no longer contain interfering or late eluting peaks; and all chromatograms are free of the large solvent peak tailing associated with the ACB eluent. The newly modified method allows for an improved and more versatile domoic acid analysis.
1987年，多莫酸（DA）首次在加拿大爱德华王子岛的贻贝中被发现。1991年，它又出现在加利福尼亚州蒙特雷湾的凤尾鱼和鹈鹕体内。同年晚些时候，在华盛顿州和俄勒冈州沿海的剃刀蛤和邓杰内斯蟹中也发现了多莫酸。自首次爆发以来，已开发出多种检测这种神经毒素的分析方法。在此，我们描述了对奎利姆高效液相色谱-紫外法（1991年：NRCC编号33001）中固相萃取（SPE）净化步骤的一种改进。标准的10%乙腈（MeCN）洗涤液和10% MeCN中的0.5M柠檬酸铵缓冲液（ACB）（pH = 4.5）洗脱液已被10% MeCN中的0.1M氯化钠（NaCl）洗涤液和10% MeCN中的0.5M NaCl洗脱液所取代。这种改进使该分析方法在蛤和蟹的内脏及肉样上都能同样良好地发挥作用。内脏样本的色谱图不再包含干扰峰或洗脱较晚的峰；并且所有色谱图都没有与ACB洗脱液相关的大溶剂峰拖尾现象。新改进的方法实现了更完善、更通用的多莫酸分析。
