黄海胶州湾海水中蛤毒素特征及变化规律

Pectenotoxin profile and its variation in seawater of Jiaozhou Bay, Yellow Sea,China

中文关键词: 蛤毒素  海水  液相色谱-串联质谱  胶州湾

英文关键词: Pectenotoxin  Seawater  LC-MS/MS  Jiaozhou Bay

中文摘要:

      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3 m处，每次放置4 d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1 ml 80%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 Ionization，ESI）阳离子模式。样品分析所用分离柱为Waters XTerra C18柱 (50 × 2.1 mm, 3.5 μm)，预柱为C18 (10 × 2.1 mm, 3.5 μm)。流动相A为2 mmol/L甲酸铵 、50mmol/L甲酸溶于95％的乙腈；流动相B为2 mmol/L甲酸铵、50mmol/L甲酸溶于纯水。流速为0.4 ml/min，淋洗梯度为0~11min, 35 % A ~ 100 %A;在11~16.5min, 100 % A;在16.5~17.0 min，100 % A ~35 % A。分别给出海水中蛤毒素PTX-2、PTX-2 SA、 7-epi-PTX-2 SA、 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-2 SA 和 7-epi-PTX-2 SA，不存在蛤毒素PTX-11、 PTX-12a 和 PTX-12b。海水中蛤毒素PTX-2、PTX-2 SA 与7-epi-PTX-2 SA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。

英文摘要:

      The aim of the present study was to investigate the pectenotoxin (PTX）profiles in seawater. Solid phase adsorption toxin tracking (SPATT) methods were adopted to adsorb toxins in seawater. The toxins absorption disks (TADs）containing the absorbent were hung at 3m depth in seawater at the sampling locations (36°12.428′N, 120°17.826′E) in Jiaozhou Bay of Yellow Sea from Jul. 28 to Aug. 29, 2006. After 4 days, the disks were taken out and a new disk was hung. The toxins in the resin were washed out with methanol. The methanol fraction was evaporated to dryness, then re-dissolved in 1.0 ml 80% methanol. The 80% methanol solution was analyzed on the LC-MS/MS system. The MS/MS system was equipped with an electrospray ion source (ESI) operating in positive ionization mode. Injection aliquots were separated on a Waters XTerra C18 column (50 × 2.1 mm, 3.5μm) connected to a C18 pre-column (10 × 2.1 mm, 3.5μm). The mobile phases consisted of 2mmol/L ammonium formate and 50mmol/L formic acid in 95% acetonitrile (mobile phase A) and 2mmol/L ammonium formate and 50mmol/L formic acid in water (mobile phase B). A gradient was run at 0.4ml/min from 35% A to 100% A for 11 min, followed by an isocratic period for 5.5 min at 100% A. The gradient was returned to 35% A over 0.5 min and left to equilibrate at 35% A for 3 min before the next injection.Chromatograms of PTX-2, PTX-2 SA, 7-epi-PTX-2 SA, PTX-11, PTX-12a and PTX-12b of extracts of seawater were given respectively. PTX-2, PTX-2 SA and 7-epi-PTX-2 SA were found in seawater of this area. The highest levels of PTXs (PTX-2, PTX-2 SA,and 7-epi-PTX-2 SA) in seawater were found on Aug. 1st, 2006. From Aug. 1st to Aug. 29th, the levels of PTX-2 and PTX-2 SA decreased. PTX-11, PTX-12a, and PTX-12b were not found in seawater of Jiaozhou Bay， Yellow Sea.