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1.
建立了水产饲料中甲基睾丸酮的超高效液相色谱-串联质谱分析方法。具体优化了检测过程中提取液体积分数、提取时间、固相萃取柱、洗脱液浓缩方式、质谱条件和流动相组成等对加标回收率有影响的主要因素。样品经40%甲醇水提取,提取液经C18固相萃取柱净化,用超高效液相色谱-串联质谱仪测定。甲基睾丸酮的质量浓度在0.50~10.00μg/L线性良好,该方法的检出限为2.00μg/kg,定量限为5.00μg/kg。本方法适用于大批量饲料中的甲基睾丸酮的快速检测。  相似文献   

2.
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。  相似文献   

3.
《畜禽业》2018,(12)
探索了应用QuEChERS-超高效液相色谱-串联谱联用技术同时检测饲料中8种抗氧化剂的定性定量方法。优化饲料样品的前处理方法,研究最适宜的方法提取饲料中合成抗氧化剂,利用QuEChERS前处理方法,梯度洗脱使用水和乙腈流动相运行,电喷雾离子源电离、正负离子多反应监测模式质谱对检测对象进行分析。方法检出限为0. 005~0. 1mg/kg,定量限0. 01~0. 2 mg/kg;检测结果为饲料中的8种抗氧化剂显现出良好的线性关系(r~2=0. 9921~0. 9992),在低、中、高三个不同浓度梯度的添加平均加标回收率为76. 2%~102. 8%,方法能适合检测抗氧剂的需要。  相似文献   

4.
建立了亲水作用色谱-串联质谱法(HILIC-MS/MS)检测渔用配合饲料中左旋肉碱含量的方法。样品用超纯水超声提取,提取液稀释后经HILIC色谱柱分离,以乙腈和乙酸铵(含0.15%甲酸)溶液为流动相梯度洗脱,三重四级杆串联质谱多反应监测(MRM)方式扫描,外标法定量。结果表明,左旋肉碱在0.2~100 ng/mL范围线性良好(r>0.999);检出限0.5μg/kg,定量限1.5μg/kg。在20、50和100 mg/kg添加水平下,回收率为75.2%~111%,相对标准偏差RSD为3.4%~9.9%(n=6)。该方法前处理简单、快速,定性定量准确,适合于渔用配合饲料中左旋肉碱的准确定性定量。  相似文献   

5.
建立一种测定水产品中利福平药物残留的超高效液相色谱—串联质谱检测方法。样品用乙腈—二氯甲烷(6∶4,体积比)提取剂提取,通过100 mg C18+100 mg PSA分散固相萃取净化,以3 mmol/L乙酸铵溶液(含0.05%甲酸)和乙腈为流动相进行梯度洗脱,采用电喷雾离子源正离子多反应监测模式测定,内标法定量分析。检测结果显示,利福平在1~20μg/kg质量浓度内呈良好的线性关系,相关系数r≥0.9986,方法检出限为0.3μg/kg,定量限为1.0μg/kg,对罗非鱼、凡纳滨对虾、中华鳖进行加标回收试验,回收率为90.17%~101.07%,相对标准偏差为3.11%~7.66%,该方法简单、快速、准确,适用于水产品中利福平残留的确证和定量分析,为监管利福平药物的违规使用提供便捷、有效的技术支持。  相似文献   

6.
为了准确评估渔业生态环境中的孔雀石绿(MG)及其代谢产物隐性孔雀石绿(LMG)的残留状况,建立了3种渔业环境基质(水体、底泥和底泥-水体混合物)中MG和LMG的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。通过考察不同前处理方法对不同基质中MG和LMG回收率的影响,优化仪器性能,确定了色谱和质谱分析条件。具体方法是:水体过滤后采用PRS固相萃取柱进行净化、富集;底泥采用乙腈-二氯甲烷(1∶1,v/v)提取,再旋蒸、富集;底泥-水体混合物用二氯甲烷提取后,采用PRS固相萃取柱净化、富集。采用Thermo C18色谱柱对待测物进行分离,以乙腈-0. 2%乙酸铵(1∶1,v/v)为流动相洗脱,电喷雾-多反应正离子监测模式监测,内标法定量。结果表明,3种不同基质中的MG和LMG在1~8 ng/m L范围内线性显著,其相关系数r~2值大于0. 999;加标回收率分别为90. 0%~104. 2%、79. 9%~90. 3%和74. 1%~86. 3%,相对标准偏差为3. 3%~5. 8%、4. 9%~8. 6%和3. 2%~8. 3%; MG的检出限(LOD,S/N=3)分别为0. 24 ng/L、0. 02μg/kg和0. 06μg/kg,定量限(LOQ,S/N=10)分别为0. 79 ng/L、0. 07μg/kg和0. 21μg/kg; LMG的检出限(LOD,S/N=3)分别为1. 14 ng/L、0. 17μg/kg和0. 12μg/kg,定量限(LOQ,S/N=10)分别为4. 72 ng/L、0. 56μg/kg和0. 39μg/kg。该法可应用于渔业环境中MG及LMG的定性定量检测,具有较好的实用性。  相似文献   

7.
建立了3龄仿刺参和幼参体腔液中皮质醇的超高效液相色谱—串联质谱的检测方法。样品采用乙腈-0.2%甲酸溶液均质振荡、超声提取,用Captiva EMR-Lipid固相萃取柱净化,BEH C-18色谱柱分离,采用超高效液相色谱—串联质谱仪进行测定。试验结果表明,方法的检出限为0.11μg/L,定量限为0.35μg/L,在空白样品中分别添加皮质醇质量浓度为20、40、100μg/L,其回收率均为77%~105%,该方法基质干扰小,准确,易操作,能够满足仿刺参体腔液中痕量皮质醇的测定。  相似文献   

8.
《畜禽业》2021,(8)
目的建立动物源性食品(猪肉、猪肝、禽肉)中喹乙醇代谢物3-甲基喹噁啉-2-羧酸(MQCA)高效液相色谱-串联质谱法。方法样品通过偏磷酸水解提取MQCA,MAX固相萃取柱净化。采用0.1%甲酸溶液和甲醇溶液作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对MQCA的定量离子和定性离子进行监测。结果该方法10 min完成目标化合物的分析,MQCA在0.5~2μg/kg浓度范围内呈良好的线性关系,MQCA在0.5μg/kg、1μg/kg和2μg/kg添加水平的回收率为75.4%~105%,相对标准偏差小于7.96%(n=6),方法检出低限为0.1μg/kg。结论该方法前处理耗时短、灵敏度高、回收率高,适用于动物源性食品(猪肉、猪肝、禽肉)中喹乙醇代谢物3-甲基喹噁啉-2-羧酸(MQCA)的残留测定。  相似文献   

9.
采用超高效液相色谱-串联质谱(UPLC-MS/MS)法,检测水产品中7种喹诺酮药物残留。选取青鱼、泥鳅和南美白对虾样品,用1%甲酸-乙腈超声提取后,经Oasis? Prime HLB固相萃取柱一步净化,氮吹浓缩,最后用10%甲醇复溶,0.1%甲酸水和纯甲醇作为流动相进行梯度洗脱,流量为0.3 mL/min,在电喷雾-多反应监测正离子模式下,7种喹诺酮(QNs)均采用内标法定量。结果表明,7种QNs药物在1.0~100.0μg/kg范围内,呈良好的线性关系,相关系数(R2)均高于0.998 000。7种QNs在空白样品中添加浓度分别为5.0,1.0和20.0μg/kg时,在青鱼中回收率为92.71%~105.31%,泥鳅中回收率为92.31%~109.38%,南美白对虾中回收率为92.31%~106.76%。该方法具有较好的准确度和重复性。按照特征离子色谱峰信噪比(S/N)=3计算得出,7种QNs检出限为0.01~0.34μg/kg,定量限为0.04~0.87μg/kg。指出,该方法操作简便,灵敏度高,准确度好,适合大批量水产品中7种喹诺酮药物残留的检测分析。  相似文献   

10.
建立了固相萃取净化气相色谱-串联质谱(GC-MS/MS)测定稻田水产品中26种持久性有机污染物残留的检测方法。样品经二氯甲烷-正己烷(1∶1,V/V)混合溶剂超声提取,由氨基固相萃取柱净化,采用气相色谱分离,在选择反应监测模式(SRM)下测定。结果表明,26种目标物在1~500μg/L范围内线性关系良好,相关系数R~2均大于0.997,方法的检测限(LOD)为0.20~1.00μg/kg,定量限(LQD)为0.60~3.00μg/kg。26种目标物在鲤(Cyprinus carpio)和克氏原螯虾(Procambarus clarkii)空白样品中不同添加水平的平均回收率为70.6%~115.0%,相对标准偏差(RSD)为3.29%~10.90%。该方法适用于稻田水产品中26种持久性有机污染物的测定。[中国渔业质量与标准,2020,10(4):45-56]  相似文献   

11.
The environmental processes associated with variability in the catch rates of bigeye tuna in the Atlantic Ocean are largely unexplored. This study used generalized additive models (GAMs) fitted to Taiwanese longline fishery data from 1990 to 2009 and investigated the association between environmental variables and catch rates to identify the processes influencing bigeye tuna distribution in the Atlantic Ocean. The present findings reveal that the year (temporal factor), latitude and longitude (spatial factors), and major regular longline target species of albacore catches are significant for the standardization of bigeye tuna catch rates in the Atlantic Ocean. The standardized catch rates and distribution of bigeye tuna were found to be related to environmental and climatic variation. The model selection processes showed that the selected GAMs explained 70% of the cumulative deviance in the entire Atlantic Ocean. Regarding environmental factors, the depth of the 20 degree isotherm (D20) substantially contributed to the explained deviance; other important factors were sea surface temperature (SST) and sea surface height deviation (SSHD). The potential fishing grounds were observed with SSTs of 22–28°C, a D20 shallower than 150 m and negative SSHDs in the Atlantic Ocean. The higher predicted catch rates were increased in the positive northern tropical Atlantic and negative North Atlantic Oscillation events with a higher SST and shallow D20, suggesting that climatic oscillations affect the population abundance and distribution of bigeye tuna.  相似文献   

12.
13.
Previously, we reported 10 PEGE types of 85 tilapia Streptococcus agalactiae(GBS), which shifted from Streptococcus iniae in China, by using PEGE method. Presently, larger and more representative tilapia GBS were isolated, for the ?rst time in China, to characterize their serotypes and genetic diversities more precisely than had done before. 168 GBS strains were distributed in ?ve provinces of China, in which Guangdong, Guangxi and Hainan were the major ones, holding36.9%(62/168), 37.5%(63/168) and 19.6%(33/168), respectively. Serotypes, Ia, Ib and III, were observed in these strains and the most predominant one was Ia(95.2%), which mainly distributed in Guangdong, Guangxi and Hainan. Ia initially occurred in 2009, it shoot up to 32.1% in 2010,but decreased to 16.1% in 2011 before went up to 45.2% in 2012. Ib sporadically occurred during2007–2011, III onlyoccurred in 2012. 14 different PFGE types, including 4 new types(N, O,P and Q), were observed, in which B, D, F and G were the predominant types, holding 83.9%(141/168) of the total GBS strains. Ia corresponded to 11 PFGE types(A–H, N–P), in which type D predominated(51%). Ib represented 3 genotypes(I, J and Q) and III harbored only 2genotypes(N and F). Type N and Fsynchronously presented in Ia and III. In summary, the genetic diversity of tilapia GBS varied by serotypes and changed with geographical locations and years.Although Iastillpredominated, new rareserotypeIII alreadyoccurred in China.  相似文献   

14.
In this experiment, a feeding trial was performed to determine the effects of fructooligosaccharide (FOS) on growth performance, digestive enzyme activity and immune response of Japanese sea bass, Lateolabrax japonicus juveniles (initial weight 38.3 ± 0.5 g), and the fish were examined following feeding with six levels of FOS (0, 0.5, 1, 2, 4 and 6 g/kg) for 28 days. Significant enhancement of weight gain (WG) and specific growth rate (SGR) was found in fish fed 1 g/kg FOS incorporated diets (p < .05), while the feed conversion ratio (FCR) in the 1, 2 g/kg FOS groups reduced significantly compared with the control (p < .05). Besides, the crude lipid in the 4, 6 g/kg FOS groups increased significantly compared with the control (p < .05). On the other hand, the erepsin and lipase activities significantly elevated in intestine of fish fed 2 g/kg FOS (p < .05) and the lysozyme activity in serum of fish fed 2 g/kg FOS were significantly higher than that in the control (p < .05). Moreover, the alkaline phosphatase activities in serum of fish fed 0.5, 1, 2 g/kg FOS were significantly higher than in control (p < .05). Regression analysis showed that the relationships between dietary FOS levels and either SGR, FCR, erepsin or lysozyme activities were best expressed by regression equations, and the optimal inclusion levels are 1.37, 1.80, 3.06, 3.11, 1.93 and 1.80 g/kg for SGR, FCR, erepsin, lipase, lysozyme and total superoxide dismutase activities, respectively. Overall, this study revealed that FOS incorporated diets could beneficial for L. japonicus culture in terms of increasing the growth, digestion and immune activities. Under the present experimental condition, the optimal supplementary level of FOS in the diet of L. japonicus is 1–3 g/kg.  相似文献   

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16.
The purpose of this work was to evaluate the suitability of a method based on the presence of two restriction sites (for Hae III and Hindf I) in the mitochondrial NADH dehydrogenase subunit 5 (mt ND5) gene to identify Scomber species. The evaluation was performed on 144 reference and market samples by sequencing of the entire 505-bp fragment of the mt ND5 gene and of a 464-bp fragment of the Kocher fragment of the cytochrome b gene (mt Cytb). Sequence analysis of any of the two fragments allows the identification of each of the four Scomber species, but S. japonicus and S. colias had the same restriction sites at the ND5 amplicon and would not have been differentiated by this analysis. Similarly, loss of the Hae III site in some S. scombrus individuals would have misidentified them as not being Scomber. All the market products were correctly labeled except one acquired in Spain labeled as originating in the Atlantic and containing S. japonicus.  相似文献   

17.
Growth hormone (GH) and reproduction: a review   总被引:5,自引:0,他引:5  
Interaction between growth and reproduction occurs in many vertebrates and is particularly obvious at certain stages of the life cycle in fish. Endocrine interactions between the gonadotropic axis and the somatotropic axis are described, the potential role of GH being emphasised. A comparative analysis of these phenomena in mammals, amphibians and fish, suggests a specific role of GH in the physiology of puberty, gametogenesis and fertility. It also shows the original contribution made by studies on the fish model in this field of investigations.  相似文献   

18.
Two gonadotropins (GtH; Qa and Qb) were purified by gel filtration and ion exchange chromatography from the pituitaries of Indian walking catfish (Clarias batrachus). The presence of GtH during purification was assessed by in vitro oocyte maturation and in vivo steroidogenic activity, and their identities were determined by elution profiles, molecular weight, biological activities and yield. The molecular weights of Qa and Qb were 37 and 42 kDa, respectively, and composed of distinct subunits (Qa: 20 and 14 kDa and Qb: 26 and 18 kDa). Polyclonal antibodies raised against Qa immunostained Qa, Qb and pituitary GtH cells. A competitive Qa‐ELISA was developed whose sensitivity was 6.25 ng mL?1 (1.25 ng well?1) with intra‐ (3.5%) and inter‐ (12.4%) assay coefficients of variation. Displacement curves parallel to the standard were obtained with plasma and pituitary extracts of catfish, Qb and carp GtHII. The assay was validated by measuring the plasma Qa levels after LHRH treatment and in relation to ovarian growth in the female catfish during different reproductive phases. Based on the results, Qa and Qb corresponded to fish LH and FSH respectively. The findings will increase the knowledge of the mechanisms controlling fish reproduction and identification of sensitive phases in fish in captivity for hormonal manipulation.  相似文献   

19.
Tetrahymena is a protozoan parasite, which infects guppy, Poecilia reticulata Peters, and causes substantial economical losses in commercial farms worldwide. Studies of guppy infected by Tetrahymena require standardized infection protocols. The LD50 for Tetrahymena infection of guppies by intraperitoneal (IP) injection was calibrated, and the level obtained was 946 parasites per fish. Guppy infection with Tetrahymena by immersion, imitating the natural route of infection via the integument, was studied under normal or stress conditions. Exposure to cold and netting (CNI) and to cold only (CI) followed by immersion exposure to 10 000 Tetrahymena per mL resulted in 22.5% and 19.2% mortality, respectively, as compared to 14.2% and 10% in groups that were netted only (NI) or non‐stressed (I). Histopathology revealed that immersion infection resulted in a systemic infection. Lysozyme levels, measured 3 weeks after infection, were significantly higher in the CNI group (288 μg per mg protein) compared with CI‐, NI‐ and I‐treated groups (94.5, 64 and 62.3 μg mg?1, respectively). There was no evident parasite immobilization activity in body homogenates, suggesting no development of acquired immunity. Re‐infection by IP injection revealed no increase in protection in any of the treatment groups, mortality range of 56.3–75%, higher than in the non‐exposed control (40.6% mortality).  相似文献   

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