超高效液相色谱串联质谱法对水产品中硝基呋喃代谢物的测定

建立了使用Waters UPLC Xevo TQ超高效液相色谱串联质谱仪检测水产品中4种硝基呋喃代谢物的分析方法。匀浆后的样品在酸性环境下水解,并用2-硝基苯甲醛衍生16h,经磷酸氢二钾提取,LMS固相萃取小柱净化后,在三重四极杆多反应监测模式下进行测定。方法采用同位素内标法定量,四种代谢物的检出限(LOD)均低于0.25μg·kg-1,线性范围在0.5μg·L~(-1)到10μg·L~(-1)间,相关系数大于0.99。在0.5、1.0和5μg·kg-1浓度下分别进行添加回收试验(n=5),回收率在75.2%~123.3%之间,相对标准偏差(RSD)小于9.4%。     

An improved method for extraction of sorghum polymeric protein complexes

A method for fractionating sorghum proteins using extraction solvents and techniques designed to obtain polymeric protein structures (especially disulfide linked) was developed. Extraction and separation conditions were optimized in terms of completeness of protein extraction, sample stability, and analytical resolution. After pre-extraction of albumins and globulins, a 3-step sequential procedure involving no reducing agents was applied to ground whole sorghum flour. The three fractions obtained represented proportionally different protein polymer contents and molecular weight distribution as evidenced by comparative size exclusion chromatography. Protein composition also varied among the extracts with differences in kafirin composition and non-kafirin proteins detected in the fractions by RP-HPLC and SDS-PAGE analysis. The ability to quantify and further characterize sorghum polymeric protein complexes will be useful for additional studies linking protein structures with functionality and digestibility and variations for these properties within diverse sorghum germplasm.     

基质分散萃取-高效液相色谱法对菠菜中噻虫胺残留的检测

研究确立了乙腈为分散萃取溶剂,以羧基化双壁碳纳米管(DWCNTs-COOH)和石墨化碳黑(GCB)为基质分散材料的菠菜(Spinacia oleracea L.)样品中噻虫胺残留基质分散萃取前处理方法,建立并优化了乙腈等度洗脱的HPLC残留样品外标定量方法。结果表明,优化色谱条件下,噻虫胺标准样品的色谱保留时间为6.258 min,在0.05~100 mg/L范围内与对应色谱峰积分面积线性响应良好,回归方程为y=4.948 2x-1.316 9(R~2=0.999 7),噻虫胺在菠菜样品中0.1、0.5和5.0 mg/kg 3个水平的添加回收率均在85%以上,各添加水平的相对标准偏差均小于7%,该色谱条件下仪器检出限为0.052 7μg/L,方法的最低检测量为0.015 mg/kg。表明该残留样本前处理方法和样品检测方法简便、高效、经济、可靠,可满足噻虫胺在菠菜中的残留定量检测要求。     

用酶法制备藏羊血食用蛋白粉的研究

采用四因素三水平正交试验,对藏羊血制备食用蛋白的工艺进行了分析。经分析食用蛋白粉水解最佳条件为：酶解用酶量4.5g,酶解温度为46℃,酶解时间为7.5h,酶解的pH值为10.5,活性炭作用于水解液时由室温升至80℃所需最佳时间为6～8min。     

Nanostructured liquid crystalline particle assisted delivery of 2,4-dichlorophenoxyacetic acid to weeds,crops and model plants

Routine agricultural practices are heavily dependent on the use of surfactants, many of which are toxic to humans and detrimental to the environment. In proof of concept work we have previously shown the potential of nanostructured liquid crystalline particles (NLCP) to safely interact with plant leaf cuticular surfaces with minimal impact on epicuticular waxes. Here we demonstrate the use of NLCP to effectively deliver the auxin herbicide 2,4-dichlorophenoxyacetic acid (2,4-D) to plant leaves in laboratory and field studies. In the laboratory, the physiological stress responses of lupin, Lupinus angustifolius (L.) (Fabaceae) towards NLCP spray applications were shown to be much reduced in comparison with application of two common surfactants. Phytotoxicity assays of 2,4-D loaded NLCP were used to validate the herbicidal effects on Arabidopsis thaliana (L.) Heynth. (Brassicaceae) and established a similarity with that of surfactant assisted 2,4-D delivery when tested at a concentration of 0.1%. Field trials were conducted to test the efficacy of NLCP-assisted delivery of 2,4-D in comparison with commercial surfactants for the control of the invasive weed wild radish, Raphanus raphanistrum (L.) (Brassicaceae), in wheat, Triticum aestivum (L.) (Poaceae) crop fields. Compared against Estercide 800, a commercially available 2,4-D formulation, NLCP assisted delivery of 2,4-D was effective at low concentrations of 0.03% and 0.06%. The crop yield remained similar for all the tested concentrations and formulations of 2,4-D loaded NLCP and Estercide 800. This is the first report to directly show that, as an alternative to conventional methods, NLCP can be used under both laboratory and field conditions to successfully delivery an agrochemical.     

高效液相色谱法测定海洋生物中牛磺酸的含量

[目的]建立牛磺酸的高效液相色谱分析方法,并通过该方法测定不同海洋生物中牛磺酸的含量。[方法]应用邻苯二甲醛(OPA)柱前衍生法,研究流动相比例、流速、衍生剂比例、衍生时间等因素对牛磺酸检测的影响。[结果]当牛磺酸∶OPA=1∶2,衍生时间2 min,流动相乙腈∶水=15∶85,流速为0.5 mL/min,检测波长为360 nm时,牛磺酸浓度为10~400μg/mL时具有良好的线性关系(R~20.99),平行样品的相对标准偏差为2.9%~7.4%。利用该方法检测不同海产品中牛磺酸的含量,所选择的海洋贝类、甲壳类、鱼类中均含有牛磺酸,其中海瓜子中含量最高,达11.2 mg/g。不同组织比较,鱼肉中牛磺酸含量较高,而鳃中较低。[结论]该研究结果丰富了海洋生物中牛磺酸含量的数据,为进一步研究牛磺酸在不同组织中的合成机制提供了参考。     

Ovarian mixed germ-cell tumor comprising mature teratoma and embryonal carcinoma in a four-toed hedgehog (Atelerix albiventris)

This report describes the clinical and histopathological characteristics of a rare mixed germ-cell tumor comprising teratoma and embryonal carcinoma in the left ovary of a 10-month-old four-toed hedgehog, with chief complaints of loss of appetite and lethargy. Laparotomy revealed a swollen left ovary with small disseminated peritoneal nodules, and bilateral ovariohysterectomy was performed. The left ovary had a mature teratoma with well-differentiated fat, bone, cartilage, salivary gland, trachea, keratin cyst, and nervous tissues, and an embryonal carcinoma consisting of poorly-differentiated epithelial cells arranged in tubular, alveolar, or solid patterns. Immunohistochemically, the embryonal carcinoma cells were positive for placental alkaline phosphatase and c-KIT. This is the first case of mature teratoma with embryonal carcinoma in the ovary of a hedgehog.     

Variation among stallions in sperm quality after single layer centrifugation

Although single layer centrifugation (SLC) selects robust spermatozoa from stallion semen, the effect of individual variation has not been studied in detail. The objective of this study was to determine the variation among stallions in the effects of SLC on sperm quality during cooled storage for up to 48 hr. Semen samples from seven stallions (18 ejaculates) were split, with one portion being used for SLC and the other serving as a control (CON). Sperm quality (kinematics, reactive oxygen species (ROS) production, membrane integrity (MI) and chromatin integrity) were analysed at 0, 24 and 48 hr using computer-assisted sperm analysis and flow cytometry. Sperm quality was better in SLC than in CON at all timepoints, especially chromatin integrity and MI (p < .0001 for both), and some categories of ROS production (e.g. proportion of live hydrogen peroxide negative spermatozoa, p < .0001), but the degree of improvement varied among stallions and type of ROS (p < .05–p < .0001). Total and progressive motility were also better in SLC samples than in CON at 24 and 48 hr (p < .0001), although the effect on sperm kinematics varied. The interaction of treatment, time and stallion was not significant. In conclusion, sperm quality was better in SLC samples than in CON, although there was considerable individual variation among stallions. The improvement in sperm quality, particularly in chromatin integrity, was clearly beneficial, and therefore the use of this technique would be warranted for all stallion semen samples.     

超高效液相色谱法测定饲料中斑蝥黄和β-阿朴-8’-胡萝卜素酸乙酯含量方法的研究

为有效快速测定饲料中斑蝥黄和β-阿朴-8’-胡萝卜素酸乙酯含量,饲料经甲醇、正己烷和乙酸乙酯混合液萃取后,在氮气保护下浓缩,用甲基叔丁基醚-乙腈溶液复溶,注入超高效液相色谱仪中进行测定。结果表明:斑蝥黄浓度为1.25~10.0μg/mL,β-阿朴-8’-胡萝卜素酸乙酯为2.50~20.0μg/mL线性关系良好;斑蝥黄和β-阿朴-8’-胡萝卜素酸乙酯的检测限为0.06 mg/kg,定量限为0.20 mg/kg。斑蝥黄5个添加水平的平均回收率为72.8%~82.8%,相对标准偏差(RSD)为0.41%~1.06%;β-阿朴-8’-胡萝卜素酸乙酯5个添加水平的平均回收率为72.0%~82.8%,RSD为0.46%~1.41%。说明该方法简便、快速、灵敏度高、准确度好,适用于测定饲料中斑蝥黄和β-阿朴-8’-胡萝卜素酸乙酯含量。