广州市售四种贝类重金属含量分析及评价

采用电感耦合等离子体原子发射光谱法,对广州市售4种食用贝类体内Cd、Cr、Cu、Pb、As进行检测,分析其重金属污染状况,对其质量安全进行评价。结果表明,缢蛏、波纹巴非蛤、丽文蛤和菲律宾蛤仔,Cd、Cr、Cu、Pb含量均低于国家无公害标准,而As含量均超过国家无公害标准。分析认为,广州市售4种贝类已受到一定程度的As污染,应引起重视。     

利用电压敏感荧光染料测定贝体中的麻痹性贝毒

麻痹性贝毒(paralytic shellfish poisoning, PSP)是分布最广、危害最大的赤潮毒素,可阻断钠离子通道从而抑制动作电位的形成导致动物体中毒。以膀胱癌移行细胞T24为实验材料,采用电压敏感荧光染料bis-oxonol,根据PSP毒素GTX2,3对藜芦定诱导细胞去极化的抑制作用,建立了一种麻痹性贝毒电压敏感荧光染料检测法。实验结果显示,在2～100 ng·mL-1范围内,PSP毒素GTX2,3可显著改变培养体系的荧光强度,GTX浓度与荧光强度之间存在很好的线性关系。市售贝类PSP毒素检测结果表明,此方法测定结果与小鼠法基本一致,但灵敏度更高,说明根据GTX浓度与荧光强度之间的线性关系可实现对样品中PSP毒素的快速检测。利用电压敏感荧光染料测定贝体中的麻痹性贝毒是一种非常有潜力的贝毒快速筛查方法。     

高效液相色谱-串联质谱法同时测定贝类中22种农药残留

建立了高效液相色谱-三重四极杆质谱（HPLC-MS/MS）同时测定贝类中22种农药残留的分析方法。样品经含0.1%（v/v）甲酸的乙腈提取，N-丙基乙二胺（PSA）和石墨化碳黑（GCB）净化，然后采用ACE UltraCore 2.5 SuperC18柱（100 mm×2.1 mm，2.5 μm）分离，以甲醇-0.1%（v/v）甲酸水溶液为流动相梯度洗脱，流速为0.4 mL/min，柱温为35 ℃，然后以电喷雾电离（ESI）源，在多反应监测（MRM）、正离子模式下，采用三重四极杆质谱检测。22种农药在各自的线性范围内线性关系良好，相关系数均大于0.997，检出限为0.1~0.3 μg/kg，定量限为0.3~1.0 μg/kg。在3个添加水平下，22种农药的平均回收率为65.2%~109.4%，相对标准偏差为1.3%~15.2%（n=6）。该方法操作简单，快速，准确度高，灵敏度高，可用于贝类中22种农药残留的同时检测。     

How the marine biotoxins affect human health

Several marine microalgae produce dangerous toxins very damaging to human health, aquatic ecosystems and coastal resources. These Harmful Algal Blooms (HABs) in recent decades seem greatly increased regarding frequency, severity and biogeographical level, causing serious health risks as a consequence of the consumption of contaminated seafood. Toxins can cause various clinically described syndromes, characterised by a wide range of symptoms: amnesic (ASP), diarrhoetic (DSP), azaspirazid (AZP), neurotoxic (NSP) and paralytic (PSP) shellfish poisonings and ciguatera fish poisoning. The spread of HABs is probably a result of anthropogenic activities and climate change, that influence marine planktonic systems, including global warming, habitat modification, eutrophication and growth of exogenous species in response to human pressures. HABs are a worldwide matter that requests local solutions and international cooperation. This review supplies an overview of HAB phenomena, and, in particular, we describe the major consequences of HABs on human health.     

Quantification of domoic acid in shellfish tissues by pressurized capillary electrochromatography

A method was developed to quantify domoic acid (DA), the chemical responsible for amnesic shellfish poisoning (ASP), by pressurized CEC (pCEC). The effect of different experimental conditions on the separation of DA and matrix solutes, such as the content of ACN in mobile phase, pH and concentration of buffer, supplementary pressure and applied voltage, were investigated. Under the optimal conditions, the pCEC method separated DA from shellfish matrices within 6 min. By using supplementary pressure, bubble formation in the capillary column was completely suppressed. The method was repeatable, sufficient accurate and sensitive for rapid screening of DA in shell seafood.     

麻痹性贝类毒素标准样品的研制

将麻痹性贝类毒素阳性的新鲜扇贝去壳后取贝肉,经过匀浆,冷冻干燥等步骤制备成冻干粉,然后进行均匀性和稳定性检验,结果表明,制备后的样品均匀,稳定,满足标准样品的要求。以多家实验室定值的方式对该标准样品进行定值,定值结果为（589±42）MU／g（k=-2）。该标准样品可用于麻痹性贝类毒素检测过程的方法验证与质量控制。     

液相色谱-串联质谱法同时测定贝类中大田软海绵酸、鳍藻毒素、蛤毒素和虾夷扇贝毒素

建立了同时测定贝类中大田软海绵酸(okadaic acid, OA)及其衍生物鳍藻毒素(dinophysistoxin-1, DTX-1)、蛤毒素(pectenotoxin-2, PTX-2)和虾夷扇贝毒素(yessotoxin, YTX)的液相色谱-串联质谱分析方法。样品经甲醇提取,固相萃取柱净化,C18色谱柱分离,经含甲酸和甲酸铵的乙腈-水溶液为流动相梯度洗脱,选择反应监测(SRM)模式检测,正、负离子切换扫描,基质标准校正,外标法定量。结果表明,OA、DTX-1和YTX的线性范围为2.0～200.0 μg/L,定量限(以信噪比(S/N)≥10计)为1.0 μg/kg; PTX-2的线性范围为1.0～100.0 μg/L,定量限为0.5 μg/kg;几种化合物的添加平均回收率为83.1%～105.7%,相对标准偏差(RSD)为3.16%～9.29%。成功应用本法对黄海灵山湾海域采集的贝类样品进行了分析,发现部分样品中含有大田软海绵酸、鳍藻毒素、蛤毒素和虾夷扇贝毒素。     

HPLC determination of domoic acid in shellfish based on magnetic molecularly imprinting polymers

A magnetic molecularly imprinting polymer for domoic acid was fabricated. Synthesis conditions were optimized. The polymer particles have high magnetization for rapid magnetic separation. The apparent maximum absorption amount and dissociation constant of the polymer were 1,600?µg?g^?1 and 20.6?µg?mL^?1, respectively. The polymer retained 90% of adsorption amount after 5 times of repeated use. It was used as an adsorbent for purification and HPLC detection of domoic acid in shellfish with a detection limit of 0.050?µg?g^?1. Thus, the polymer could be applied to the sample pretreatment of aquatic products.     

养虾废水经贝类滤食净化后池塘主要水环境因子的变化分析

2001-2002年浙江省宁海县采用封闭式内循环养殖模式养殖南美白对虾，每公顷对虾养殖产量达到12090kg，取得了显著的经济效益，为对虾的成功养殖开辟了一条有效途径．该模式在对虾养殖过程中会产生大量的养殖废水，而养殖废水主要是富营养化问题．结合养殖新模式的运行，从COD、磷酸盐、亚硝酸盐、硝酸盐、氨氮和悬浮物几项理化因子指标的变化情况，对贝类的净化能力作出分析评价，为海水围塘虾贝的综合养殖提供理论依据．     

Analysis of the characteristic PSP profiles ofPyrodinium bahamense and several strains ofAlexandrium by HPLC based on ion-pair chromatographic separation, post-column oxidation, and fluorescence detection

Summary A sensitive HPLC method for determination of paralytic shellfish poisoning (PSP) based on ion-pair chromatographic separation of PSP toxins, post-column oxidation with periodic acid, and fluorescence detection has been used to determine toxin profiles ofPyrodinium bahamense and several strains ofAlexandrium. The HPLC chromatograms revealed clear differences betweenPyrodinium bahamense andAlexandrium strains. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996.