UPLC—MS／MS法测定奶粉中烟酸醮含量     

郝刚  ;俞蕴莉  ;顾炳仁 《中国乳业》2014,(11):54-58

建立一种专属、灵敏、快速的超高效液相色谱串联质谱（UPLC—MS／MS）测定奶粉中烟酸含量的方法。烟酸提取后经强阳离子交换（SCX）固相萃取柱净化,采用BEH—C18超高效液相色谱柱、20mmol／L乙酸水溶液-乙腈（体积比为20：80）流动相分离,以电喷雾离子源正离子方式进行多反应监测（MRM）。试验结果表明,1～500ng／L浓度范围内,烟酸呈良好的线性关系,相关系数R=O．9995。低、中、高3个烟酸浓度添加水平的回收率为78．2％～904％,相对标准偏差小于7％。奶粉中烟酸的检出限为0．25ug／g,定量限为O．75ug／g。采用所建方法对市售6批奶粉进行测定,烟酸含量均符合规定。所建方法适合奶粉中烟酸的含量测定。  相似文献   

Phage and MLVA Typing of Salmonella Enteritidis Isolated from Layers and Humans in Belgium from 2000–2010, A Period in which Vaccination of Laying Hens was Introduced     

M. Heyndrickx  G. Rasschaert  S. Bertrand  C. Wildemauwe  P. Wattiau  H. Imberechts  L. Herman  R. Ducatelle  S. Van Weyenberg  K. De Reu 《Zoonoses and public health》2014,61(6):398-404

The aim of the study was to characterize isolates of Salmonella enterica serovar Enteritidis (S. Enteritidis) obtained from humans and layer farms in Belgium collected during 2000–2010. Three periods were compared, namely (i) before implementation of vaccination (2000–2004), (ii) during voluntary vaccination (2005–2006) and (iii) during implementation of the national control program (NCP) for Salmonella including mandatory vaccination against S. Enteritidis (2007–2010). The characteristics compared across time periods were distributions of phage type and multiple‐locus variable number tandem‐repeat assay (MLVA). While PT4 and PT21 were predominantly isolated in Belgium in layers and humans before 2007, a significant reduction of those PTs was observed in both populations in the period 2007–2010. The relative proportion of PT4b, PT21c and PT6c was found to have increased considerably in the layer population since 2007. In the human population, PT8, PT1 and the group of ‘other’ PTs were more frequently isolated compared to the previous periods. When comparing the proportion of the predominant MLVA types Q2 and U2, no significant difference was found between the layer and human population in the three periods and between periods within each category (layer and human). A significant difference in isolate distribution among MLVA clusters I and II was found between human and layer isolates recovered during Period 3 and in the human population between Period 1 and 3. Results suggest that the association between S. Enteritidis in layers and the occurrence of the pathogen in humans changed since implementation of the NCP in 2007.  相似文献   

Discrimination of the natal origin of young-of-the-year Allis shad (Alosa alosa) in the Garonne–Dordogne basin (south-west France) using otolith chemistry     

J. Tomás  S. Augagneur  E. Rochard 《Ecology of Freshwater Fish》2005,14(2):185-190

Abstract –  The otolith composition of age 0+ Allis shad ( Alosa alosa ) captured in two rivers in the Gironde system in south-west France, the Dordogne and the Garonne, was analysed to establish the natal origin of the fish. Inductively coupled plasma mass spectrometry analyses were used to take measurements of 15 isotopes, among which Co, Fe, Sr and Rb were the most important elements in the discrimination process. It was possible to reclassify each sampled fish into its natal river basin (Garonne or Dordogne) with a high degree of accuracy. Linear discriminant analysis correctly reclassified 91.1% of the Garonne samples and 87.8% of the Dordogne samples (mean success in reclassification in 20 runs ± 1 SD: 89.21 ± 8.6%). Artificial neural networks correctly reclassified 90.1% of the Garonne samples and 81.2% of the Dordogne samples (mean success in reclassification after 1000 training cycles ±1 SD: 85.6 ± 9.1%). Using these tools the present results show that it is possible to assign a natal origin to juvenile shad that hatched in the Dordogne–Garonne basin based on the trace elements in the otolith.  相似文献   

Endotoxin Structures in the Psychrophiles Psychromonas marina and Psychrobacter cryohalolentis Contain Distinctive Acyl Features     

Charles R. Sweet  Giancarlo M. Alpuche  Corinne A. Landis  Benjamin C. Sandman 《Marine drugs》2014,12(7):4126-4147

Lipid A is the essential component of endotoxin (Gram-negative lipopolysaccharide), a potent immunostimulatory compound. As the outer surface of the outer membrane, the details of lipid A structure are crucial not only to bacterial pathogenesis but also to membrane integrity. This work characterizes the structure of lipid A in two psychrophiles, Psychromonas marina and Psychrobacter cryohalolentis, and also two mesophiles to which they are related using MALDI-TOF MS and fatty acid methyl ester (FAME) GC-MS. P. marina lipid A is strikingly similar to that of Escherichia coli in organization and total acyl size, but incorporates an unusual doubly unsaturated tetradecadienoyl acyl residue. P. cryohalolentis also shows structural organization similar to a closely related mesophile, Acinetobacter baumannii, however it has generally shorter acyl constituents and shows many acyl variants differing by single methylene (-CH₂-) units, a characteristic it shares with the one previously reported psychrotolerant lipid A structure. This work is the first detailed structural characterization of lipid A from an obligate psychrophile and the second from a psychrotolerant species. It reveals distinctive structural features of psychrophilic lipid A in comparison to that of related mesophiles which suggest constitutive adaptations to maintain outer membrane fluidity in cold environments.  相似文献   

Metabolomic Tools for Secondary Metabolite Discovery from Marine Microbial Symbionts     

Lynsey Macintyre  Tong Zhang  Christina Viegelmann  Ignacio Juarez Martinez  Cheng Cheng  Catherine Dowdells  Usama Ramadan Abdelmohsen  Christine Gernert  Ute Hentschel  RuAngelie Edrada-Ebel 《Marine drugs》2014,12(6):3416-3448

Marine invertebrate-associated symbiotic bacteria produce a plethora of novel secondary metabolites which may be structurally unique with interesting pharmacological properties. Selection of strains usually relies on literature searching, genetic screening and bioactivity results, often without considering the chemical novelty and abundance of secondary metabolites being produced by the microorganism until the time-consuming bioassay-guided isolation stages. To fast track the selection process, metabolomic tools were used to aid strain selection by investigating differences in the chemical profiles of 77 bacterial extracts isolated from cold water marine invertebrates from Orkney, Scotland using liquid chromatography-high resolution mass spectrometry (LC-HRMS) and nuclear magnetic resonance (NMR) spectroscopy. Following mass spectrometric analysis and dereplication using an Excel macro developed in-house, principal component analysis (PCA) was employed to differentiate the bacterial strains based on their chemical profiles. NMR ¹H and correlation spectroscopy (COSY) were also employed to obtain a chemical fingerprint of each bacterial strain and to confirm the presence of functional groups and spin systems. These results were then combined with taxonomic identification and bioassay screening data to identify three bacterial strains, namely Bacillus sp. 4117, Rhodococcus sp. ZS402 and Vibrio splendidus strain LGP32, to prioritize for scale-up based on their chemically interesting secondary metabolomes, established through dereplication and interesting bioactivities, determined from bioassay screening.  相似文献   

微波消解-石墨炉原子吸收光谱法测定人参中铅和镉     

张冠英  李青  郭金芝  王蕴馨  马莹  姜楠 《人参研究》2014,(2):38-39

目的建立一种快速准确的微波消解-石墨炉原子吸收光谱法测定人参中铅和镉的含量。方法采用微波消解对样品进行前处理,应用石墨炉原子吸收光谱法测定人参中铅和镉的含量。结果铅在0μg/L~40μg/L范围,镉在0μg/L~3μg/L范围具有良好的线性,相关系数均大于0.999,检出限分别为3.6μg/kg和0.42μg/kg,相对标准偏差(RSD)为9.11%和4.70%,加标回收率在93.3%~106.7%之间。结论该方法简便快速、准确灵敏,适用于测定人参中铅和镉的含量。  相似文献   

基于液质联用技术的坛紫菜甘油-3-磷酸胁迫响应分析     

唐欣怡  赵佳丽  陈娟娟  骆其君  陈海敏  杨锐  张鹏 《核农学报》2022,36(4):788-794

甘油-3-磷酸作为渗透压调节物红藻糖苷的合成前体物,参与藻类抗逆应答过程。为了解坛紫菜的抗逆机制,通过超高效液相色谱-质谱联用技术(UPLC-MS)建立甘油-3-磷酸的定量分析方法,分析非生物(温度、盐度和干出)胁迫下的甘油-3-磷酸响应规律。结果表明,温度胁迫1 h后,甘油-3-磷酸的含量快速变化,当温度高于23℃时,甘油-3-磷酸含量与胁迫温度成正比,而在12℃低温下,甘油-3-磷酸的含量反而下降;盐度胁迫促使甘油-3-磷酸的含量快速上升,且高盐胁迫下的变化显著高于低盐环境;而短时间1 h干出胁迫后的甘油-3-磷酸含量略有上升(1.19倍,与对照组相比),但随着干出时间继续延长,甘油-3-磷酸含量总体呈现下降趋势。温度、盐度和干出胁迫后的坛紫菜进行恢复培养后,甘油-3-磷酸含量均趋于对照组水平。综上可知,甘油-3-磷酸可快速响应环境胁迫,这为坛紫菜红藻糖苷抗逆机制的多层次研究奠定了基础。  相似文献   

铁皮石斛枫斗加工前后差异成分比较     

刘鹏飞  范蓓  刘湘丹  杨洋  卢聪  佟立涛  孙晶  王凤忠 《核农学报》2022,36(12):2412-2418

铁皮石斛(Dendrobium officinale Kimura et Migo)的传统功效为益胃生津、滋阴清热,在降血糖方面具有较好的作用。前期研究发现,与铁皮石斛鲜条相比,枫斗的α-葡萄糖苷酶抑制率更高,且枫斗中化学成分种类丰富。为明确铁皮石斛枫斗与鲜条的差异性成分,阐明铁皮石斛加工成枫斗的科学内涵,本研究利用超高效液相色谱-四级杆串联飞行时间质谱仪(UPLC-QTOF-MS)在正离子模式下采集二者的代谢物信息,通过主成分分析、偏最小二乘判别分析等算法挖掘差异性化合物,并利用质谱碎片、数据库比对等方式鉴定差异性成分,最后采用聚类分析方法研究差异性成分在铁皮石斛枫斗和鲜条中的含量变化规律。经过筛选和鉴定共得到16种差异性化合物,其中柚皮素、4,4'-二羟基-3,5-二甲基联苄、诺比林A、石斛酚等12种黄酮、联苄类化合物在枫斗中含量较高,而α-亚麻酸、L-苯丙氨酸、草质素等4种脂肪酸、氨基酸类化合物在鲜条中含量较高,这些差异性成分可能是潜在的铁皮石斛枫斗降血糖功能成分。本研究结果为阐明铁皮石斛枫斗降血糖物质基础提供了数据支撑,对进一步促进铁皮石斛精深加工具有重要意义。  相似文献   

ICP-MS法测定沙棘籽油中13种微量元素     

张荣 《国际沙棘研究与开发》2014,(1):10-13,17

沙棘籽油样品经微波消解处理,采用电感耦合等离子体质谱法测定所得样品溶液中铁、硒、锌、钾、钠、钙、镁、铜、锰、铅、砷、汞、镉等13种微量元素的含量。使用动态反应池技术消除了多原子离子对部分被测元素的干扰。方法快速准确、灵敏度高,加标回收率在95.5%~102.8%之间,相对标准偏差小于3%。  相似文献   

兽用止痢、止泻中草药制剂的质量检测及制备(英文)     

蔡璐  ;蒋秀全  ;杨何  ;蔡一鸣 《农业科学与技术》2014,(7):1180-1182

[目的]制订止痢、止泻兽用中草药制剂的质量检验标准。[方法]分别采用理化鉴别和紫外分光光度计的定性检测对比试验。[结果]蒸馏水法检测的最大吸收峰峰值相差大于1 nm;0.9%盐酸法和60%乙醇法得出最大吸收峰的峰值相差小于1 nm,次吸收峰的峰值差别也均小于1 nm。[结论]选用0.9%盐酸法和60%乙醇法作为兽用止痢、止泻中草药制剂的质量检测标准。  相似文献