气相色谱-质谱法测定海水及贝类中的丙烯酸丁酯

本文采用有机溶剂萃取的提取方法,利用气相色谱-质谱选择离子法,建立了海水及贝类中丙烯酸丁酯的检测方法.该方法在0.01 ～ 10.00 mg/L范围内具有良好的线性,线性相关系数为0.9 994;在海水和贝类样品中检出限(S/N=3)分别为0.001 mg/L和0.01mg/kg;在加标回收率试验中,海水中丙烯酸丁酯的平均回收率为104.2％,贝类样品中丙烯酸丁酯的平均回收率为91.8％;方法相对标准偏差(n=6)小于7.53％.通过实际样品的测定,表明本方法满足海水和贝类样品中丙烯酸丁酯检测分析的要求.     

水产品中丙酸睾酮激素的同位素稀释气相色谱-质谱法分析

针对鱼虾等水产品中的丙酸睾酮残留,以诺龙-D3为内标研究了气相色谱-质谱(GC/MS)检测技术.捣碎匀浆后的样品中加入内标诺龙-D3和饱和NaCl溶液混匀后,叔丁基甲醚超声提取,-80℃冷冻20 min脱脂,SilicaSPE柱净化和柱前三甲基硅烷化后,进行GC/MS分析.选择离子监测(SIM)模式下,根据丙酸睾酮和诺...     

气相色谱-质谱法测定水产品中氟胺氰菊酯残留量

本文建立了水产品中氟胺氰菊酯残留量的气相色谱-质谱测定方法。样品经正己烷-丙酮（体积比2：1）超声提取、冷冻除脂、中性氧化铝固相萃取柱净化后,用气相色谱-质谱法进行测定和确认,外标法定量。在优化实验条件下,氟胺氰菊酯在10．0～400．0μg·L^-1范围内线性关系良好,相关系数为0．9999,检出限为2．0μg·kg^-1,定量限为4．0μg·kg^-1。在4．0、8．0和40．0μg·kg^-1加标水平下,鲤（Cyprinus carpio）、草鱼（Ctenopharyngodon ideUus）和凡纳滨对虾（Penaeus vannamei Boone）可食部分为基质的平均回收率为87．92％～98．37％,相对标准偏差为0．96％～4．97％。该方法操作简单、灵敏度高、净化效果理想、重珊陛好,可满足水产品中氟胺氰菊酯的定性定量检测的要求。     

气相色谱-质谱法测定动物源性水产品中16种除草剂

本研究建立了动物源性水产品中16种除草剂的凝胶色谱-固相萃取净化、气相色谱-质谱分析方法.结果显示,样品通过二氯甲烷-乙酸乙酯混合溶液提取、凝胶渗透过滤及固相萃取柱净化,采用气相色谱-质谱联用方法测定,选择离子监测、外标法定量.二甲戊乐灵、草净津在4-200 μg/L浓度范围内,其余14种在2-100μg/L浓度范围内与其响应值呈良好的线性关系,相关系数(一不低于0.9970.扑灭津、阿特拉津、特丁津、西玛津、敌草净、扑草净、莠灭净、异丙甲草胺定量限均为1.0 μg/kg;乙草胺、甲草胺、丁草胺、丙草胺、环草津、西草净定量限均为1.5 μg/kg;二甲戊乐灵、草净津定量限均为2.0 μg/kg.平均回收率为67.2％-103.0％,相对标准偏差为5.1 ％-9.5％.研究表明,该方法重现性好,回收率高,在精密度、准确度方面能满足残留检测要求,适用于水产品中16种除草剂残留的同时检测.用此方法检测了海参、牡蛎、扇贝等水产品中除草剂残留量,检出率最高的是莠灭净,其次是阿扑草净、特拉津、西草净、乙草胺,同时为进一步探讨除草剂污染对水产品质量安全的影响奠定基础.     

液相色谱-串联质谱法测定水产品中孔雀石绿的残留量

建立了液相色谱-串联质谱测定水产品中孔雀石绿及其代谢物残留的检测方法。样品经乙酸铵盐溶液和乙腈提取,经二氯甲烷萃取,PRS阳离子交换柱净化,然后选用电喷雾离子源,在正离子、多反应监测方式模式下进行定性,以内标法进行定量。方法的检出限为0.10μg·kg-1,工作曲线的线性范围为0.10~4.00μg·kg-1。在添加浓度为0.10~4.00μg·kg-1的范围内,孔雀石绿和隐色孔雀石绿的平均回收率均分别为83.4%和95.0%,相对标准偏差分别为6.23%和6.74%。     

固相萃取-气相色谱-质谱联用法测定水产品中邻苯二甲酸酯的残留量

建立了测定水产品中常见的6种邻苯二甲酸酯类化合物（ PAEs）的气相色谱-质谱（GC-MS）分析方法。样品经环己烷：乙酸乙酯（V/V,1∶1）混合溶液超声提取,用乙腈饱和的正己烷除脂,再用正己烷饱和的乙腈反提,过PAE30006-C固相萃取小柱净化,用1%乙酸乙酯的正己烷淋洗,再用正己烷：乙酸乙酯（V/V,1∶1）混合溶液洗脱,洗脱液浓缩后,正己烷定容,供GC-MS测定。结果显示：6种邻苯二甲酸酯类化合物（ PAEs）在10-5000 ng/mL的线性范围内,相关系数在0．9992-0．9998,线性良好,检出限（ LOD ）在0．62-2．96μg/kg,定量限（ LOQ）在2．0-9．0μg/kg。选择罗非鱼样品为测试对象,按照10μg/kg、50μg/kg和100μg/kg 的添加量做加标回收试验,平均回收率在70．5%-105．4%之间,相对标准偏差在3．78%-7．57%之间;选用南美白对虾、草鱼、锯缘青蟹、大黄鱼和牡蛎样品对此方法进行验证,在添加浓度为50 ug/kg的水平上进行加标回收实验,6种PAEs的平均加标回收率在71．5%-102．5%之间,相对标准偏差在3．25%-7．86%之间。该方法提取效率高,净化效果好,可操作性强,符合水产品中药物残留检测的要求。     

气相色谱-质谱法测定甲壳类水产品中4-己基间苯二酚残留

研究建立了甲壳类水产品中4-己基间苯二酚(4-hexylresorcinol,4-HR)残留量的固相萃取-气相色谱-质谱检测方法。样品采用乙酸乙酯提取,硅胶柱净化,乙酸乙酯洗脱,气相色谱-质谱测定,外标法定量。4-HR的响应值与其质量浓度在0.05~10μg/m L范围内的线性关系良好,相关系数为0.9 997;0.05~1 mg/kg添加浓度的日内和日间平均回收率为76.8%~102%,相对标准偏差为2.43%~7.65%;检出限为0.01 mg/kg,最低定量限为0.05 mg/kg。该方法适用于甲壳类水产品中4-HR残留的检测。     

气相色谱质谱法同时测定水产品中 8 种雌激素类化合物

应用气相色谱-质谱建立了同时检测水产品中辛酚、壬酚、双酚A、己烯雌酚、雌酮、17肛雌二醇、17a-乙炔雌二醇和雌三醇8种雌激素的方法.样品经乙酸乙酯提取,HLB小柱净化,经七氟丁酸酐衍生后用电子轰击电离源在SIM模式下进行检测.结果表明,8种激素化合物在DB.1.MS柱上能得到良好的分离,色谱峰出峰尖锐,没有杂峰干扰.本方法检出限为0.3～1.O μg/kg.在空白样品中添加水平为1.0～5.0 μg/kg范围内,平均回收率为81%～108%,相对标准偏差(RSD)为6.7%～11.7%.     

气相色谱-质谱法检测鱼肉中MS-222残留

本文建立了鱼肉中MS-222残留GC-MS检测方法.鱼肉样品经乙腈提取,氮吹浓缩,盐酸溶液引导MS-222电离,Waters Oasis MCX固相萃取柱净化后,气相色谱-四极杆质谱检测.方法检出限为2.5 μg·kg-1、定量限为5.0 μg·kg-1;0.0025～1.0 μg·mL-1范围内线性关系良好（R≥0.9996）;MS-222浓度范围在5.0～ 100.0 μg·kg-1的鱼肉加标样,日内和日间平均回收率为78.4％～91.2％,相对标准偏差为3.62％ ～9.49％.结果表明,该检测方法适用于低浓度水平鱼肉中MS-222残留检测.     

气相色谱—质谱法测定水产品中己烯雌酚的不确定度分析评定

依据测量不确定度评定与表示理论,从标准溶液、样品称量、样品定容、标准曲线、样品测定和测量仪器6个方面,对气相色谱—质谱法测定水产品中己烯雌酚的不确定度进行分析和评定。结果表明,标准曲线拟合和样品测量重复性这两个分量对测量结果的不确定度贡献较大,这为减少测量不确定度,提高测量准确度提供改进方向。以平均值报告水产品中己烯雌酚含量为7.58μg/kg时,扩展不确定度为2.20μg/kg。     

Differences in food composition between territorial and aggregative juvenile crimson sea bream Evynnis japonica

ABSTRACT:   Food composition, fork length and condition factor of juvenile crimson sea bream Evynnis japonica were examined for two behaviorally distinct types of fish inhabiting a nursery ground. Studies were carried out from March to September 1996 at Morode Cove, Ehime Prefecture, Japan. One type of fish is solitary and territorial and the other type is aggregative. The food compositions of the two types of fish were different. Solitary fish foraged mainly on Gammaridea and Caprellidea (benthic organisms), and Copepoda (planktonic organisms); while aggregative fish foraged mainly on Copepoda, Appendiculata and Cladocera (planktonic organisms). These findings suggest that when we study food composition of E. japonica , it is imperative to consider whether the samples used for the analyses are from solitary (territorial) fish. Solitary fish showed significantly greater fork length and condition factor than aggregative fish, suggesting that the former will have a greater fitness value than the latter.     

液质联用法检测海水中氯霉素的含量

应用液质联用仪测定海水中氯霉素的含量。水样经乙酸乙酯萃取、浓缩,以1 mL50%的甲醇-水溶液定容,采用液相色谱-三重四级杆串联质谱仪、多反应监测扫描模式（MRM）检测和氘代氯霉素内标法定量。海水中氯霉素检测方法的线性范围是0.10～10.0ng.mL-1,检出限为0.04μg.L-1,定量限为0.10μg.L-1,加标浓度在线性范围内时,回收率大于90%。试验证明：该方法比较稳定,适用于检测海水中氯霉素的含量。     

罗非鱼HSP70(tHSP70)蛋白的生物信息学分析、真核表达及质谱鉴定

运用生物信息学技术分析罗非鱼热休克蛋白70(tilapia heat shock protein,tHSP70)的理化特性、糖基化位点、跨膜区域、蛋白的细胞定位及信号肽与虹鳟等其他动物HSP70的相似性,以人工合成cDNA为模板,通过聚合酶链式反应扩增其完整CDS,并将此DNA片段与真核表达载体pGAPZa-A连接,构建pGAPZa-HSP70表达质粒,在毕赤酵母GS115中表达tHSP70蛋白,对表达上清液进行SDS-PAGE及Western-blotting分析后,采用Ni²⁺IDA层析脱盐纯化目的蛋白,并对所表达的蛋白进行糖基化PAS染色鉴定。对表达的蛋白进行SDS-PAGE后,将所获得的非预定大小(约100 ku)条带进行电离飞行时间质谱鉴定,并确定其蛋白种类。结果表明:tHSP70所含氨基酸数量为640,分子量为70 274.5 u,等电点为5.49。在哺乳动物网织红细胞(体外)的半衰期为30 h,在酵母内半衰期大于20 h,而在大肠杆菌内的半衰期也大于10 h,不稳定指数为36.64,脂肪族指数为85.58。可能分别含有6个N-和O-糖基化位点,所克隆tHSP70基因与目的基因完整编码区序列完全一致,所构建的pGAPZa-HSP70质粒能在GS115中成功表达,诱导表达上清液经SDS-PAGE及Western-blotting分析后发现,除70 ku目的蛋白外,还出现一条100 ku条带。经糖基化PAS染色证明,此100 ku蛋白可能是HSP70糖基化的结果,且能被人的兔抗HSP70抗体识别,质谱鉴定证明该条带即是tHSP70蛋白。本研究所表达tHSP70蛋白为后续罗非鱼细胞学及抗原提呈等免疫学研究奠定了基础。     

GC/MS法同时测定水产品中氯霉素、氟甲砜霉素及甲砜霉素残留量

建立了气相色谱-负离子化学电离源质谱同时测定水产品中氯霉素(CAP)、氟甲砜霉素(FF)和甲砜霉素(TAP)残留量的方法。通过优化色谱条件,实现了氯霉素、甲砜霉素及氟甲砜霉素三甲基硅(TMS)衍生物的良好分离,检测模式采用选择离子检测(SIM),监测离子为:氯霉素(m/z376、378、466、468),氟甲砜霉素(m/z339、341、429、431)及甲砜霉素(m/z409、411、499、501),分别选择466、339、409作为定量离子。方法建立的基质添加标准曲线,有效地消除了基体效应的影响,其衍生物的峰面积与其浓度在CAP为2.0～200.0ng/ml,FF和TAP在5.0～200.0ng/ml时呈良好线形关系,线性相关系数均大于0.998。基质加标实验表明,方法的准确度和精密度满足水产品中药残检测的要求。CAP的测定低限为0.3μg/kg,FF和TAP的测定低限为1.0μg/kg。     

Oyster greening by outdoor mass culture of the diatom Haslea ostrearia Simonsen in enriched seawater

Oyster greening was first described in the seventeenth century as a natural phenomenon. However, it has recently been discovered that the diatom Haslea ostrearia Simonsen causes greening by synthesis of a blue pigment designated as ‘marennine’. This phenomenon, which involves massive proliferation of H. ostrearia in oyster ponds, was not understood or controlled by oyster farmers in the Marennes‐Oléron region (Atlantic coast of France). As greening oysters improved their market value, they tried to develop empirical methods to guarantee oyster fattening and improve profits. In this context, the present study investigated the feasibility of mass culture of diatoms outdoors in 10‐m³ ponds, using enriched seawater. Different biotic and abiotic parameters were monitored daily to determine the influence of the day–night temperature range. After 8 days, H. ostrearia was the dominant diatom species (66%), reaching a mean cell concentration of 2 × 10⁵ cell mL^?1 and a marennine concentration of 3.4 mg L^?1. Although intensive greening was obtained, further studies are required to optimize the production stages before this technology can be transferred to oyster farmers.     

Effects of body size and water temperature on food consumption and growth in the sea cucumber Apostichopus japonicus (Selenka) with special reference to aestivation

To investigate the effects of body size and water temperature on feeding and growth in the sea cucumber Apostichopus japonicus (Selenka), the maximum rate of food consumption in terms of energy (C_maxe; J day^?1) and the specific growth rate in terms of energy (SGRe; % day^?1) in animals of three body sizes (mean±SE) – large (134.0±3.5 g), medium (73.6±2.2 g) and small (36.5±1.2 g) – were determined at water temperatures of 10, 15, 20, 25 and 30°C. Maximum rate of food consumption in terms of energy increased and SGRe decreased with increasing body weight at 10, 15 and 20°C. This trend, however, was not apparent at 25 and 30°C, which could be influenced by aestivation. High water temperatures (above 20°C) were disadvantageous to feeding and growth of this animal; SGRe of A. japonicus during aestivation was negative. The optimum temperatures for food consumption and for growth were similar and were between 14 and 15°C, and body size seemed to have a slight effect on the optimal temperature for food consumption or growth. Because aestivation of A. japonicus was temperature dependent, the present paper also documented the threshold temperatures to aestivation as indicated by feeding cessation. Deduced from daily food consumption of individuals, the threshold temperature to aestivation for large and medium animals (73.3–139.3 g) was 24.5?25.5°C, while that for small animals (28.9–40.7 g) was between 25.5 and 30.5°C. These values are higher than previous reports; differences in sign of aestivation, experimental condition and dwelling district of test animals could be the reasons.     

固相微萃取‒气质联用法测定鱼肉中土臭味素和2-甲基异莰醇

采用顶空固相微萃取法建立了以顺式-十氢-1-萘酚为内标物、气相色谱质谱法测定鱼肉中土臭味素和2-甲基异莰醇的定性定量测定方法.考察了鱼肉中土臭味素和2-甲基异莰醇提取和定量方法,优化了顶空固相微萃取条件,并通过实际样品的测定,考察方法的适应性.结果显示,在0.1～10.0μg/L范围内,土臭味素和2-甲基异莰醇峰面积与...     

福建南日岛东岱村北部海域夏秋冬海水水质营养状况分析评价

2012-2013年,根据夏秋冬三个季度3个航次海水水质的监测结果,对福建南日岛东岱村北部海域夏秋冬海水水质营养状况进行分析与评价。结果表明,南日岛东部东岱村北部海域海水水质良好,无机氮、化学需氧量及石油类符合国家一类海水水质标准,无机磷则在2013年2月航次监测中达到三类海水水质标准,海区富磷现象明显。总体而言,该海域海水处于健康状态,能够满足野生坛紫菜生长要求。     

凝胶渗透色谱-气相-质谱测定鲸皮脂中的多氯联苯

建立了一种测定鲸皮脂中多氯联苯(PCBs)前处理的改良方法,即将皮脂样品分别经超声波萃取、GPC净化和浓缩等处理后,用GC-MS测定.结果显示,该方法加标回收率为73%～118%,精密度为4.1%～9.7%,检出限在0.19～1.07 ng · g-1之间.该方法操作简单,净化效果好、准确性高、重复性强,适合鲸皮脂中PCBs含量的分析测定.