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采用固相萃取的方法提取海水中的蛤毒素(Pectenotoxins,PTXs)。从2006年7月28日～8月29日,将含有吸附剂的吸附盘片置于黄海胶州湾取样点(36°12.428′N,120°17.826′E)水面以下3m处,每次放置4d后取出。吸附盘片中的蛤毒素用甲醇洗脱,洗脱液蒸发浓缩近干,用1ml80%甲醇溶解,然后以液相色谱-串联质谱分析。串联质谱采用电喷雾离子原(ElectroSpray Ioniza-tion,ESI)阳离子模式。样品分析所用分离柱为Waters XTerraC18柱(50×2.1mm,3.5μm),预柱为C18(10×2.1mm,3.5μm)。流动相A为2mmol/L甲酸铵、50mmol/L甲酸溶于95%的乙腈;流动相B为2mmol/L甲酸铵、50mmol/L甲酸溶于纯水。流速为0.4ml/min,淋洗梯度为0～11min,35%A～100%A;在11～16.5min,100%A;在16.5～17.0min,100%A～35%A。分别给出海水中蛤毒素PTX-2、PTX-2SA、7-epi-PTX-2SA、PTX-11、PTX-12a和PTX-12b的质谱图。结果发现,这一海域海水中存在蛤毒素PTX-2、PTX-2SA和7-epi-PTX-2SA,不存在蛤毒素PTX-11、PTX-12a和PTX-12b。海水中蛤毒素PTX-2、PTX-2SA与7-epi-PTX-2SA之和的最大峰值出现在8月1日。然后,蛤毒素浓度逐渐降低。
Solid phase extraction (SPE) was used to extract the gelatins (PTXs) from seawater. From July 28 to August 29, 2006, the adsorption disk containing the adsorbent was placed 3m below the water surface of the Jiaozhou Bay sampling site (36 ° 12.428’N, 120 ° 17.826’E) in the Yellow Sea for 4 days After removing. The plate of toxin was eluted with methanol. The eluate was evaporated to near dryness, dissolved in 1 ml of 80% methanol and analyzed by liquid chromatography-tandem mass spectrometry. Tandem mass spectrometry uses electrospray ionization (ESI) cation mode. The separation column used for sample analysis was a Waters XTerra C18 column (50 × 2.1 mm, 3.5 μm) with a precolumn of C18 (10 × 2.1 mm, 3.5 μm). Mobile phase A was 2mmol / L ammonium formate and 50mmol / L formic acid was dissolved in 95% acetonitrile. Mobile phase B was 2mmol / L ammonium formate and 50mmol / L formic acid was dissolved in pure water. A flow rate of 0.4 ml / min, a raffinate gradient of 0 to 11 min, 35% A to 100% A, 11 to 16.5 min, 100% A, 100% A to 35% A at 16.5 to 17.0 min. The mass spectra of seawater-soluble toxin PTX-2, PTX-2SA, 7-epi-PTX-2SA, PTX-11, PTX-12a and PTX- As a result, it was found that the soxotoxins PTX-2, PTX-2SA and 7-epi-PTX-2SA were present in the seawater of this area, and no phoximin PTX-11, PTX-12a and PTX-12b were present. The maximum peak value of the sum of the sea toxins PTX-2, PTX-2SA and 7-epi-PTX-2SA appeared on August 1. Then, the concentration of the toxin gradually decreased.