罗丹明B在金鱼(Carassius auratus)组织中的蓄积及消除规律

采用水体暴露方法,研究金鱼(Carassius auratus)肝脏、肾脏、腮、肌肉和椎骨对不同质量浓度(5mg/L和15mg/L)罗丹明B的蓄积规律,采用注射染毒然后在清水中饲养的方法研究鱼体组织罗丹明B的消除规律。结果表明:罗丹明B质量浓度为5mg/L和15mg/L时,分别在第15天和12天达到吸收平衡。蓄积达到平衡时罗丹明B在高、低染毒质量浓度中的最大和最小蓄积系数分别出现在肝脏和肌肉,最大蓄积系数分别为16.14和7.37,最小蓄积系数分别为0.97和0.77。注射染毒后罗丹明B消除研究结果表明:随时间延长罗丹明组织浓度逐步下降,第9天接近平衡。不同组织中消除速度表现:肾脏>肌肉>椎骨>腮>肝脏。生物半衰期t1/2在组织中的差异表现为:肝脏>腮>椎骨>肾脏>肌肉。     

刺参体内铝的富集和消除规律研究

目的研究铝在刺参体内的富集和消除规律。方法选取体重为(50±10) g的刺参暴露于铝浓度分别为50、150、300μg/L的海水中进行富集实验,分别在第0、1、3、5、7、10、15、21、30 d取样检测分析。富集实验结束后,放入自然海水中开始消除实验,分别在第1、3、7、14、21、35、45 d取样检测分析。结果3个实验组刺参体壁中铝的蓄积量范围为10.0～18.2mg/kg、富集系数范围为53.2～160、最终消除率范围为67.0%～78.6%;纵肌中铝的蓄积量范围为32.2～60.0mg/kg、富集系数范围为189～582、最终消除率范围为84.7%～88.2%;呼吸树中铝的蓄积量范围为69.2～120mg/kg、富集系数范围为365～1143、最终消除率范围为77.9%～86.4%;消化道中铝的蓄积量范围为78.7～275mg/kg、富集系数范围为865～1275、最终消除率范围为74.8%～86.1%。结论刺参各组织铝蓄积量、富集系数随暴露时间的延长而增大,各组织对铝蓄积量和富集系数大小顺序均为消化道呼吸树纵肌体壁,消化道和呼吸树是刺参富集铝的主要器官。刺参纵肌、呼吸树和消化道对铝的蓄积量、富集系数均随暴露浓度的增大而增大,体壁对铝的蓄积量也随暴露浓度的增大而增大,但体壁对铝的富集系数随暴露浓度的增大而减小。消除实验期间,刺参体壁、纵肌、呼吸树和消化道中铝残留量随消除时间的延长而降低,呈现前期消除较快,后期逐渐平稳的趋势;消除实验结束,3个浓度组刺参中铝的最终残留量与对照组相差不大。     

采用臭氧系统净化太平洋牡蛎中的大肠杆菌

采用人工方法使太平洋牡蛎(Crassostrea gigas)体内积累的埃希氏大肠杆菌(E.coli)达到5个对数值后,放入小型臭氧净化实验系统中,通过正交试验,研究了各种环境因子对太平洋牡蛎自身净化能力的影响。经48 h净化处理后,贝肉中的E.coli减小约2～3个对数值,太平洋牡蛎的最佳净化条件为:温度15℃、换水率3次/h、贝水质量比为1:4。海水中O_3浓度为0.1～0.2mg/L时具有明显的杀菌作用。同时分析了臭氧系统处理海水的原理和影响因子,证明了臭氧系统用于净化太平洋牡蛎中的E.coli是有效的。     

超高效液相色谱-串联质谱法测定红美人中8种酚酸化合物

建立超高效液相色谱－串联质谱（ultra performance liquid chromatograph tandem mass spectrometry,UPLC-MS/MS）同时测定红美人中没食子酸、原尔茶酸、对羟基苯甲酸、绿原酸、香草酸、对香豆酸、阿魏酸、芥子酸8种酚酸化合物的方法,分析各酚酸在红美人中的组成和含量。选用2 mol/L氢氧化钠水解提取样品中游离型酚酸、游离酯型酚酸和结合酯型酚酸,提取液经固相萃取小柱净化后,采用Waters ACQUITY UPLC HSS T3色谱柱、乙腈/0.01%甲酸水流动相梯度分离,UPLC-MS/MS多反应监测模式进行测定,外标法定量。结果显示：8种酚酸在5 μg/L～5 000 μg/L浓度范围内线性关系良好（r≥0.999 1）,检出限为 0.05 μg/L～0.73 μg/L,定量限为 0.17 μg/L～2.44 μg/L,回收率为 85.7%～103.9%,重复性为0.92%～5.28%。6个产地红美人中8种酚酸均有检出,总酚酸含量在68.82 μg/g～98.96 μg/g之间,其中阿魏酸含量最高,在 38.02 μg/g～53.79 μg/g之间,绿原酸含量次之,在 15.84 μg/g～25.90 μg/g 之间;各产地红美人中的酚酸组成比例基本稳定,其中阿魏酸占比均在51.10%～57.51%,绿原酸占比均在22.29%～27.86%。     

气相色谱-质谱法同时测定草莓中7种除草剂农药残留

建立了气相色谱-质谱法(GC-MS),选择离子技术对草莓中乙草胺、西玛津、哒螨酮、禾草克、阿特拉津、扑草净、甲草胺多残留进行同时检测的方法.匀浆后的草莓试样用乙酸乙酯进行提取,提取液经滤纸过滤后收集,再浓缩蒸干,用丙酮:正己烷(30:70,V/V)溶液溶解至5ml,经Florisil固相萃取柱净化,吹干后用丙酮定容,供气相色谱-质谱联用仪进行测定.实验结果表明,除草剂在0.05～1.00 μg/ml浓度范围内,具有良好的线性响应,相关系数分别在0.9964到0.9998之间,添加浓度为0.05～1.00 μg/ml时,回收率在77.4%～125.2%之间,该方法的最低检测限为0.01 μg/g.     

地西泮在鲫鱼不同组织中的残留消除规律研究

目的 掌握地西泮在鲫鱼不同组织中的残留消除规律,合理确定休药期。方法 以鲫鱼为研究对象, 用地西泮(初始质量浓度为1 μg/L)进行药浴,分别于给药后的0.5、1、2、3、4、6、8、10、12、24、48、72、96、144、240、288、360、480、600、840、1080、1320 h对鲫鱼肌肉+皮、鳃、肝脏、肾脏、脑、心脏以及血浆等进行检测,探讨鲫鱼不同组织中地西泮药物残留消除规律,并利用WT1.4软件计算地西泮在鲫鱼体内的休药期。结果 地西泮在水产品中的代谢周期较长。肌肉＋皮组织的休药期为74 d,鳃的休药期为121 d,肝脏的休药期为174 d,肾脏的休药期为100 d,脑的休药期为78 d,心脏的休药期为45 d,血浆的休药期为106 d,结论 为保证鲫鱼质量安全和消费者健康,建议在养殖温度为20℃时,对鲫鱼单剂量(1.0 μg/L)药浴地西泮后的休药期为174 d。     

LLE-GC-MS-SIM检测白酒中9 种微量功能成分

应用液液萃取（liquid-liquid extraction,LLE）结合气相色谱-质谱-选择离子扫描（gas chromatography-mass spectrometry-selective ion monitoring,GC-MS-SIM）技术检测20 种白酒中D-柠檬烯、对伞花烃、叶绿醇、4-甲基愈创木酚、4-乙基愈创木酚、麝香草酚、异丁香酚、四甲基吡嗪及亚油酸乙酯含量。该方法回收率在81.80%～109.30%之间,精密度均小于6.00%;检测范围内,线性关系良好（R2＞0.999 0）,检出限和定量限分别为0.17～0.91 μg/L和0.58～3.04 μg/L。LLE-GC-MS-SIM法对9 种功能成分的定量检测结果表明,3 种萜烯类物质在浓香型酒样中含量较高,且山庄酒厂酒样含量普遍高于市售酒样;芝麻香型白酒中酚类物质含量最高,其中酒样W09中4 种酚类物质质量浓度高达4 301.61 μg/L;四甲基吡嗪在酱香型酒样中质量浓度为2 379.65～2 985.09 μg/L,远高于芝麻香型酒样的1 116.80～1 309.66 μg/L及浓香型酒样的245.40～555.76 μg/L;亚油酸乙酯在不同酒样中含量差异较大,除市售酒样W17、W19和W20外,其余酒样质量浓度为1 951.96～7 183.35 μg/L。     

固相萃取-HPLC法同时测定大米中甲萘威和阿特拉津

建立固相萃取-高效液相色谱二极管阵列检测器(DAD)法同时测定大米中甲萘威和阿特拉津的方法。样品经乙腈提取、净化、旋转蒸发和氮吹浓缩后,用甲醇定容至2 mL,通过XDB-C₁₈(250 mm×4.6 mm,5μm)色谱柱分离,流动相采用甲醇-水(60︰40,V/V),流速0.4 mL/min,柱温40℃,进样量5μL,在220 nm波长下测定。结果表明,在0~2.0μg/mL范围内,甲萘威和阿特拉津呈现良好线性关系,相关系数(R2)均为1.000,检出限分别为1.0μg/kg和3.0μg/kg。对0.2,0.4和0.8 mg/kg这3种不同浓度下甲萘威和阿特拉津准确度和精密度试验,回收率分别为88.3%~102.2%和87.5%~104.3%,相对标准偏差(RSD,n=6)分别为1.2%~3.3%和2.3%~4.7%。试验方法稳定性好、操作简单、灵敏度高,可满足于大米中甲萘威和阿特拉津测定。     

磺胺甲噁唑和磺胺嘧啶在青石斑鱼组织中的分布及代谢规律

通过一次性投喂各含有200 mg/kg磺胺甲噁唑（sulfamethoxazole,SMZ）和磺胺嘧啶（sulfadiazine,SDZ）的饲料,研究两种药物在青石斑鱼中各组织分布与消除规律。采用超高效液相色谱-串联质谱检测青石斑鱼各组织中SMZ和SDZ的含量,并用内标法定量。结果表明,SMZ在青石斑鱼各组织中的最大含量：肝脏、背肌、血浆、肾脏和鳃依次为827.97μg/kg、776.70μg/kg、610.29μg/L、432.14μg/kg和345.18μg/kg。SDZ在青石斑鱼各组织中的最大含量：肝脏、背肌、鳃、血浆和肾脏依次为895.30μg/kg、660.55μg/kg、431.88μg/kg、419.56μg/L和310.67μg/kg。SMZ在青石斑鱼各组织中的半衰期：肾脏、鳃、背肌、血浆和肝脏半衰期依次为26.65、21.00、20.38、18.73h和16.90h。SDZ在青石斑鱼各组织中的半衰期：肾脏、血浆、鳃、背肌和肝脏依次为31.50、27.72、24.75、21.66h和18.24h。SMZ和SDZ在青石斑鱼肝脏中半衰期最短,代谢速度最快;在肾脏中半衰期最长,代谢速度最慢。在水温（25±2）℃条件下,SMZ和SDZ各200mg/kg的剂量同时单次投喂青石斑鱼,建议休药期不低于3d。SMZ和SDZ代谢规律研究为磺胺类药物在水产品中的合理使用提供了参考。     

暂养净化及无水保活中太平洋牡蛎活力品质与呈味物质分析

为探明太平洋牡蛎(Crassostrea gigas)采捕后不同流通阶段活力品质与呈味物质的变化规律，模拟产业流通实际，将活体太平洋牡蛎进行暂养净化、诱导休眠和无水保活，并在不同时间段取样，以腺苷三磷酸(adenosine triphosphate,ATP)关联物、核苷酸能荷值(adenylate energy charge,AEC)及游离氨基酸变化分析牡蛎活力品质的变化；以呈味化合物含量结合呈味强度值评价流通过程中牡蛎风味品质变化。结果显示，采捕后运输及环境胁迫对其活力、呈味物质有显著影响，通过24 h暂养净化，牡蛎活力品质均呈明显恢复，其中ATP、AEC、游离氨基酸总量较净化前明显上升(P<0.05)，机体活力达到新水平；诱导休眠至保活流通阶段，牡蛎受到低温、缺氧胁迫需调动更多能量物质以维持机体平衡，各项活力品质指标较净化前明显降低(P<0.05)，处于稳定的较低水平。呈味化合物中，牡蛎在暂养净化后鲜甜味氨基酸增加，苦味氨基酸下降，随着保活时间的延长，呈味氨基酸缓慢下降；鲜甜味核苷酸肌苷5’-单磷酸(inosine 5’-monophosphate,IMP)、单磷酸腺苷...     

Unifying prolonged copper exposure, accumulation, and toxicity from food and water in a marine fish

The link between metal exposure and toxicity is complicated by numerous factors such as exposure route. Here, we exposed a marine fish (juvenile blackhead seabream Acanthopagrus schlegelii schlegelii) to copper either in a commercial fish diet or in seawater. Copper concentrations in intestine/liver were correlated linearly with influx rate, but appeared to be less influenced by uptake pathway (waterborne or dietary exposure). Influx rate best predicted Cu accumulation in the intestine and liver. However, despite being a good predictor of mortality within each pathway, influx rate was not a good predictor of mortality across both exposure pathways, as waterborne Cu caused considerably higher mortality than dietary Cu at a given influx rate. We show that the use of gill Cu accumulation irrespective of the exposure route as a model for observed fish mortality provided a clear relationship between accumulation and toxicity. Investigation of gill Cu accumulation may shed light on the different accumulation strategies from the two exposure pathways. This correlation offers potential for the use of branchial Cu concentration as an indicator of long-term Cu toxicity, allowing for differences in the relative importance of the uptake pathways in different field situations.     

The freshwater invertebrate Mysis relicta can eliminate chiral organochlorine compounds enantioselectively

Accumulation and elimination of chiral polychlorinated biphenyls (PCBs) and organochlorine (OC) pesticides by the opossum shrimp, Mysis relicta, was investigated to determine if zooplankton can stereoselectively process chiral OC contaminants. Concentrations and enantiomer fractions were measured within mysids over a 10-day exposure followed by a 45-day depuration period. Rapid accumulation occurred within mysids exposed to sediment contaminated with racemic chiral OC compounds at microg/g levels. Enantiomer enrichment was observed within mysids for the second-eluting enantiomer and the (-)-enantiomer of PCB 95 and trans-chlordane, respectively, after 7 days of exposure to spiked sediment, and for the second-eluting enantiomers of PCBs 91 and 183 and (-)-PCB 149 over longer time periods. Enantiomer fractions decreased with time during the depuration phase of the experiment for these compounds, showing that their elimination from mysids was stereoselective. Oxychlordane was detected in nonracemic proportions after exposure, indicating that mysids can metabolize trans-chlordane enantioselectively. Minimum elimination rates calculated were higher than biotransformation rates calculated for fish in previous studies, which have been shown to metabolize OC contaminants. This study is the first to show stereoselective processing of chiral OC contaminants by aquatic invertebrates.     

Tissue distribution and depuration kinetics of waterborne 14C-labeled light PAHs in mummichog (Fundulus heteroclitus)

Light polycyclic aromatic hydrocarbons (PAHs) of petrogenic origin are commonly found in estuaries and coastal areas. Though they are known to be toxic to fish, little is known about their uptake and tissue distribution. This paper reports on the results of a study on uptake, elimination, and tissue distribution of three waterborne 14C-labeled PAHs in the mummichog, Fundulus heteroclitus, using whole-body autoradiography. After a 24 h exposure to 1 μCi·L(-1) of 14C-naphthalene, 14C-1-naphthol, and 14C-phenanthrene, fish were transferred to clean water and tissue distribution examined after 0, 1, 3, 7, 14, and 21 days of depuration. All compounds were readily accumulated by fish and were also rapidly eliminated (t0.5 range=1.1 to 3.0 days). Most of the radioactivity in naphthalene- and phenanthrene-treated fish was found in gall bladder?liver>intestinal lumen. In naphthol-exposed fish, an important labeling of some brain areas was observed. Brain of naphthalene-exposed fish was also labeled after 24 h depuration, indicating that exposure to naphthalene may result in metabolite accumulation in the brain. This is the first study showing that naphthalene, naphthol, and/or unidentified metabolite(s) can accumulate in brain tissues, which may impair normal brain function.     

Effects of temperature on the elimination of benzocaine and acetylated benzocaine residues from the edible fillet of rainbow trout (Oncorhynchus mykiss)

The effect of temperature (7 degrees C and 16 degrees C) on the extent of accumulation and the elimination of benzocaine (BNZ) and its metabolite, acetylated benzocaine (AcBNZ), in the fillet tissue of rainbow trout was investigated. Residues were measured after bath exposure to an anesthetizing concentration of benzocaine (30 mg/l for 5 min) followed by a maintenance concentration (15 mg/l for 30 min). Immediately after exposure, the BNZ concentration in fillet tissue was approximately 27 micrograms/g at both temperatures; AcBNZ was 0.3 microgram/g at 7 degrees C and 0.6 microgram/g at 16 degrees C. The rates for elimination (alpha and beta) of BNZ and AcBNZ were not significantly different between the two temperatures. Terminal half-lives of elimination for BNZ were 1.62 h at 7 degrees C and 1.63 h at 16 degrees C; half-lives for AcBNZ were 2.36 h at 7 degrees C and 2.77 h at 16 degrees C.     

基于GC-MS鉴别活体太平洋牡蛎不同流通阶段气味特征变化

为揭示活体牡蛎在商业流通各环节风味品质变化规律，优化活品运输管理，提升牡蛎存活质量，本研究模拟太平洋牡蛎产业流通实际，采用固相微萃取-气相色谱-质谱联用技术对活体太平洋牡蛎暂养净化、诱导休眠、无水保活流通中挥发性风味物质种类及含量变化进行分析。结果显示：活体太平洋牡蛎组织中共鉴定出49种挥发性风味物质，主要由醛类、酮类、酯类、烃类、醇类、含氮含硫杂环类化合物构成；采捕后应激胁迫对其风味品质有较大影响，通过24 h暂养净化，牡蛎愉悦性风味化合物明显提升，刺激性气味化合物明显降低，脂质氧化得到明显的缓解；诱导休眠至保活流通阶段，牡蛎脂质氧化随保活流通时间的延长进一步加剧，挥发性风味物质总量呈缓慢积聚特征。气味活性值分析表明，己醛、庚醛、十一醛、(E)-2-壬烯醛、4-乙基苯甲醛、壬醛、(E)-2-癸烯醛、(E,E)-2,4-壬二烯醛、癸醛、(E)-2-辛烯醛、2-戊基呋喃、3-辛酮、2-壬酮是活体太平洋牡蛎流通中的关键风味物质，可以作为反映活体牡蛎生理状态的参考。主成分分析显示，前3个主成分累计贡献率为85.6%，可对不同流通阶段进行明显区分。研究表明，太平洋牡蛎采捕后通过暂养净化24 h...     

Reductions of Vibrio parahaemolyticus in Pacific oysters (Crassostrea gigas) by depuration at various temperatures

Consumption of raw oysters has been linked to several outbreaks of Vibrio parahaemolyticus infection in the United States. This study investigated effects of ice storage and UV-sterilized seawater depuration at various temperatures on reducing V. parahaemolyticus in oysters. Raw Pacific oysters (Crassostrea gigas) were inoculated with a mixed culture of five clinical strains of V. parahaemolyticus (10290, 10292, 10293, BE 98-2029 and 027-1c1) at levels of 10⁴⁻⁶ MPN/g. Inoculated oysters were either stored in ice or depurated in recirculating artificial seawater at 2, 3, 7, 10, 12.5, and 15 °C for 4–6 days. Holding oysters in ice or depuration of oysters in recirculating seawater at 2 or 3 °C for 4 days did not result in significant reductions (P > 0.05) of V. parahaemolyticus in the oysters. However, depuration at temperatures between 7 and 15 °C reduced V. parahaemolyticus populations in oysters by >3.0 log MPN/g after 5 days with no loss of oysters. Depuration at refrigerated temperatures (7–15 °C) can be applied as a post-harvest treatment for reducing V. parahaemolyticus in Pacific oysters.     

Accumulation of paralytic shellfish poison (PSP) and biotransformation of its components in oysters, Crassostrea gigas, fed with the toxic dinoflagellate Alexandrium tamarense

As a part of our studies on the mechanism of uptake of paralytic shellfish poison (PSP) and the kinetics of its accumulation in bivalves, oysters Crassostrea gigas were experimentally contaminated with PSP by being fed with the toxic dinoflagellate Alexandrium tamarense for 2, 4, 6, 8 and 10 days. Temporal variations in the PSP contents and their profiles in oysters during the feeding experiment were monitored by high-performance liquid chromatography (HPLC) and the toxin profile of the oysters was compared with that of A. tamarense. Toxins excreted from the infested oysters into the seawater for 2 and 10 days were recovered and analyzed by HPLC. PSP toxicity rapidly appeared in the tissues of oysters and their toxicity levels reached 0.6 (0.3), 2.2 (1.1), 1.0 (0.5), 3.4 (1.6) and 1.1 (0.5) MU/g (nmol/g) shucked meat at 2, 4, 6, 8 and 10 days, respectively. The accumulation rates of toxin, calculated from the total amount (nmol) of toxins expressed by the total cell number fed during the exposure period and the toxicity of the oysters, were 14.1, 18.7, 5.1, 14.9 and 3.2% for 2, 4, 6, 8 and 10 days. During feeding experiments, the toxin profile of oysters changed substantially, showing marked differences from the proportions found in the toxigenic dinoflagellate used as food. The toxin components in this strain existed almost exclusively as beta-epimers, which accounted for 66.3 mol% of the total. This contrasts with the case of the oysters, where the beta-epimers represented 24.8, 29.8, 25.1, 27.3 and 25.2 mol% of the total at 2, 4, 6, 8 and 10 days, respectively. The amount of gonyautoxin-1 (GTX1) accumulated in oysters increased linearly and slowly for 8 days and the maximum content of GTX1 reached 51.3 mol%. The composition of GTX group compounds recovered from the seawater in which the oysters had been reared was a little different from that within the oyster tissues.     

Temperature Effects on the Depuration of Vibrio parahaemolyticus and Vibrio vulnificus from the American Oyster (Crassostrea virginica)

ABSTRACT:  This study investigated temperature effects on depuration for reducing Vibrio parahaemolyticus and Vibrio vulnificus in American oyster ( Crassostrea virginica ). Raw oysters were inoculated with 5-strain cocktail of V. parahaemolyticus or V. vulnificus to levels of 10⁴ to 10⁵ MPN (most probable number)/g and depurated in artificial seawater (ASW) at 22, 15, 10, and 5 °C. Depuration of oysters at 22 °C had limited effects on reducing V. parahaemolyticus or V. vulnificus in the oysters. Populations of V. parahaemolyticus and V. vulnificus were reduced by 1.2 and 2.0 log MPN/g, respectively, after 48 h of depuration at 22 °C. Decreasing water temperature to 15 °C increased the efficacy of depuration in reducing V. parahaemolyticus and V. vulnificus in oysters. Reductions of V. parahaemolyticus and V. vulnificus in oysters increased to 2.1 and 2.9 log MPN/g, respectively, after 48 h of depuration at 15 °C. However, depurations at 10 and 5 °C were less effective than at 15 °C in reducing the Vibrio spp. in oysters. Extended depuration at 15 °C for 96 h increased reductions of V. parahaemolyticus and V. vulnificus in oysters to 2.6 and 3.3 log MPN/g, respectively.