基于UPLC-MS/MS同时测定猪粪便中5种兽药残留量的研究

为了建立同时测定猪粪便中二甲氧苄啶、磺胺对甲氧嘧啶、恩诺沙星、金霉素、泰乐菌素5种兽药残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法,样品经McIllvaineNa_2EDTA缓冲溶液提取,C18粉吸附杂质,HLB固相萃取小柱净化,浓缩富集后用0.1%甲酸甲醇溶液复溶,过滤上机,基质液外标法定量。结果显示,5种兽药在10~500μg/kg的质量浓度范围内线性良好,在添加浓度50~500μg/kg,平均回收率为53%~85%,RSD为1.87%~18.81%。该方法具有较好的准确度与精密度,能快速、准确测定猪粪便中5种兽药残留,为养殖环节实时监测兽药使用情况提供了技术支持。     

豆秸、花生秧和青贮玉米秸间的组合效应研究

本试验旨在研究豆秸、花生秧和青贮玉米秸间的组合效应。试验将豆秸、花生秧和青贮玉米秸分别以0∶100、20∶80、40∶60、60∶40、80∶20、100∶0比例进行两两组合,利用体外瘤胃发酵技术,分析不同组合对产气量及产气参数、pH、氨态氮、菌体蛋白的影响,计算各组合的单项组合效应值和综合组合效应值,进而筛选各饲料组合的适宜比例。结果表明：豆秸-花生秧、豆秸-青贮玉米秸、花生秧-青贮玉米秸组合在产气参数上差异显著(P<0.05),豆秸-花生秧和豆秸-青贮玉米秸均以20∶80时各产气参数最优,花生秧-青贮玉米秸以60∶40时各产气参数为最优;各组合对体外瘤胃液pH影响差异不显著(P>0.05);不同组合的氨态氮浓度差异显著(P<0.05),在39~64 mg/dL变化;豆秸-花生秧和花生秧-青贮玉米秸的菌体蛋白浓度随花生秧比例增多而增多,豆秸-青贮玉米秸的菌体蛋白浓度在两者比例为20∶80时最高。以多项组合效应评定指数评定各组合效应,豆秸与花生秧、青贮玉米秸均以20∶80的比例较为适宜,花生秧与青贮玉米秸比例以60∶40时较为适宜,综合组合效应指数均达到最大。     

Urinary and Plasma Catecholamines and Metanephrines in Dogs with Pheochromocytoma,Hypercortisolism, Nonadrenal Disease and in Healthy Dogs

Background

Diagnosis of pheochromocytoma (PC) is based on a combination of clinical suspicion, finding an adrenal mass, increased plasma, and urine concentrations of catecholamine metabolites and is finally confirmed with histopathology. In human medicine, it is controversial whether biochemically testing plasma is superior to testing urine.

Objectives

To measure urinary and plasma catecholamines and metanephrines in healthy dogs, dogs with PC, hypercortisolism (HC), and nonadrenal diseases (NAD) and to determine the test with the best diagnostic performance for dogs with PC.

Animals

Seven PC dogs, 10 dogs with HC, 14 dogs with NAD, 10 healthy dogs.

Methods

Prospective diagnostic clinical study. Urine and heparin plasma samples were collected and stored at −80°C before analysis using high‐pressure liquid chromatography (HPLC) coupled to electrochemical detection or tandem mass spectrometry were performed. Urinary variables were expressed as ratios to urinary creatinine concentration.

Results

Dogs with PC had significantly higher urinary normetanephrine and metanephrine : creatinine ratios and significantly higher plasma‐total and free normetanephrine and plasma‐free metanephrine concentrations compared to the 3 other groups. There were no overlapping results of urinary normetanephrine concentrations between PC and all other groups, and only one PC dog with a plasma normetanephrine concentration in the range of the dogs with HC and NAD disease. Performances of total and free plasma variables were similar. Overlap of epinephrine and norepinephrine results between the groups was large with both urine and plasma.

Conclusion and clinical importance

Measurement of normetanephrine is the preferred biochemical test for PC and urine was superior to plasma.     

液液萃取气相色谱法测定地表水中多氯联苯

指出了多氯联苯是一种持久性环境污染物,地表水中 PCBs液液萃取气相色谱法分析技术具有相当的代表性,以EPA的标准分析方法为基础,结合多年实验经验,对此方法内容进行了详细描述并对部分内容进行了优化,旨在为该方法的转化研究提供一些参考。     

雪糕中16种反式脂肪酸的测定

建立气相色谱测定雪糕中反式脂肪酸含量的方法.2.0 g雪糕样品中加入8 mL浓盐酸和10 mL无水乙醇进行前处理,经SP-2560毛细管色谱柱分离,气相色谱仪-氢火焰离子化检测器检测,面积归一化法计算组分含量.结果表明:在优化的色谱条件下,方法的检出限和定量限分别为0.012％和0.024％;实现了反式脂肪酸甲酯与顺式...     

Methane emissions and δ13C composition from beef steers consuming increasing proportions of sericea lespedeza hay on bermudagrass hay diets

An experiment was conducted to evaluate the effects of different proportions of ‘Au Grazer’ sericea lespedeza [SL, Lespedeza cuneata (Dum. Cours.) G. Don], a legume rich in condensed tannins (CT), on nutrient intake and digestibility, and to estimate methane (CH₄) emissions and ¹³C isotopic composition (δ¹³C_CH4) from beef steers consuming a forage-based diet. Twenty-five Angus-crossbred steers were distributed in a randomized complete block design (344 ± 48 kg initial BW), and randomly assigned to one of five treatments: 0SL, 25SL, 50SL, 75SL, and 100SL, diets containing 0%, 25%, 50%, 75%, and 100% of SL hay, respectively, mixed with ‘Tifton-85’ bermudagrass hay (Cynodon spp.). The study was carried out for two experimental periods of 21-d each. The statistical model included the fixed effect of treatment and random effects of block, experimental period, and their interaction. Apparent total tract digestibility of crude protein, neutral detergent fiber, and acid detergent fiber was linearly decreased (P < 0.001) by the inclusion of SL. No effects were observed for total CH₄ emissions per day, nor for CH₄ relative to organic matter intake or digestible organic matter with the inclusion of SL. However, emission of CH₄ in relation to intake of CT was affected by treatment (P < 0.001). A linear (P < 0.001) decrease and a quadratic effect (P < 0.001) were observed for δ¹³C of diets and gas, respectively, in which diets and enteric CH₄ with greater inclusion of SL were more depleted in ¹³C. Moreover, the difference in δ¹³C between diets and gas (Δδ¹³C) had a linear decrease (P = 0.001) with the inclusion of SL. The model developed to predict the C₃ proportions in the enteric CH₄ fitted to predicted values (P < 0.0001). Therefore, greater proportions of SL resulted in lesser CH₄ emission when CT intake was considered and the isotopic composition from enteric CH₄ was able to predict the contribution of SL in the emissions.     

双道原子荧光光谱同时测定土壤中砷、汞的方法研究

研究了土壤中总As、总Hg的同时测定方法,并对消化体系进行了筛选,利用正交试验设计法对测试条件进行了优化.建立了用王水消解样品,在10%盐酸溶液中用双道原子荧光光度计同时测定土壤中As、Hg的新方法.方法线性范围宽(As 0～200μg/L;Hg 0～10μg/L);检出限低(As 0.05μg/L;Hg 0.007μg/L);As的回收率为96.0%～101.0%,Hg的回收率为97.0%～103.7%;相对标准偏差(RSD)As为2.7%,Hg为4.5%.该方法准确、简便、快速,结果令人满意.     

无柄灵芝菌LZ02高产漆酶条件及部分酶学性质分析

【目的】 从采自新疆天山的无柄灵芝菌(G.resinaceum)中筛选获得1株高产漆酶的LZ02菌株,对其产酶条件进行优化,研究部分酶学性质。【方法】 采用单因素实验,对其产酶条件优化并研究其酶学特性,采用双向电泳检测酶蛋白。【结果】 LZ02菌株产漆酶的最佳碳源为2.5%麦麸+1%葡萄糖,最佳氮源为干酪素; Cu²⁺、Mg²⁺、Fe²⁺、 Zn²⁺和Ca²⁺的添加对LZ02产漆酶有一定的促进作用,而Co²⁺具有明显的抑制作用;藜芦醇和愈创木酚抑制产酶并使产酶高峰由第3 d推后至第9 d,添加没食子酸和ABTS对产酶影响不大,单宁酸对产酶有抑制作用。LZ02菌漆酶最适反应温度为60℃,且在80℃仍具有漆酶活性;在40℃,pH 4.0~5.0,酶活性最稳定;最适反应pH为3.0,Mn²⁺ 、Zn²⁺、 Cu²⁺ 、Ba²⁺和K⁺对酶稳定性有一定的促进作用,Co²⁺、Cd²⁺、Cr²⁺和Pb²⁺对酶的稳定性具有明显的破坏作用;对菌体及发酵液进行了双向电泳检测,测定其等电点为4.1;获得了1个纯化酶蛋白质谱序列,该蛋白与Ganoderma Lucidum来源的Laccase高度同源。【结论】 无柄灵芝菌(G.resinaceum)漆酶的合成和分泌受到营养水平、培养条件、生长阶段以及培养基中诱导剂的严格调控,木质素或木质素相关的芳香类化合物、N源和C源也能调节漆酶的合成;漆酶活性对不同种类、不同浓度的金属离子以及诱导剂的响应不尽相同,其具有较复杂的生理功能及调控机制。     

脂质分析技术及其在植物种子脂质 代谢调控研究中的应用进展

脂质是一类具有独特生理功能活性的化合物,参与调节多种植物应答非生物胁迫过程,对维持植 物组织中生理动态平衡至关重要。脂质组学（Lipidomics）自 2003 年被提出后,已迅速发展成为对脂质整体系 统分析的一门新兴学科,为传统代谢组学注入新的技术支撑,有助于阐明脂类物质在植物中的代谢调控机制。 同时,质谱成像技术因其具有无标记、非特异性、高灵敏度、多物质同时分析等优势,被广泛应用到植物组织 中各类脂质分子的空间分布研究。介绍了脂质组学和质谱成像技术的研究现状,重点综述脂质分析技术在植物 种子脂质代谢调控研究中的最新进展,特别是新兴质谱成像技术在植物种子中脂类物质的成像应用。脂质组学 和质谱成像技术作为目前多组学技术的重要补充,将为植物代谢途径和调控机制的深入探究提供新的契机。亚 微米级高空间分辨率质谱成像技术的不断发展,将进一步推动植物在空间分辨水平的脂质代谢调控网络的深入 解析和前沿应用研究。