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采用超高效液相色谱-串联质谱(UPLC-MS/MS)法,测定了凡纳滨对虾(Litopenaeus vannam ei)中氨基脲(SEM)、1-氨基-2-内酰脲(AHD)、3-氨基-2-唑烷基酮(AOZ)和5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)4种硝基呋喃类代谢物。采用2-硝基苯甲醛作为衍生化试剂,氘、碳-13、氮-15同位素标记的SEM1-3C1-5N2、AHD1-3C3、AOZ-D4和AMOZ-D5为内标物,样品经衍生、乙酸乙酯提取、正己烷净化,以甲醇0.5 mmol.L-1乙酸铵水溶液(含0.1%甲酸)为流动相进行梯度洗脱,8 m in可将4种目标化合物完全分离并测定。结果表明,4种待测物在0.4~20.0 ng.mL-1范围内线性关系良好(R〉0.999),检出限为0.03~0.15μg.kg-1。在0.5μg.kg-1、1.0μg.kg-1和2.0μg.kg-13个水平上进行加标回收试验,平均回收率为92.0%~107.3%,RSD为3.1%~8.7%。采用该法参加FAPAS国际水平测试,获得了满意的结果。 相似文献
23.
研究了多剂量混饲口灌给药方式下,诺氟沙星在草鱼体内的残留消除情况。结果显示:以每千克鱼体重10 mg连续5d混饲给药后,停药后第12天在草鱼肌肉中未检测到药物,此时血清、肝脏和肾脏中的药物浓度分别降为(0.0287±0.0015)μg/mL、(0.0181±0.0042)μg/g和(0.0369±0.0037)μg/g,均低于0.05μg/mL或0.05μg/g。因此初步建议在(19±1)℃水温条件下,以每千克鱼体重10 mg连续5 d混饲给草鱼诺氟沙星,休药期至少为最后一次给药后的12 d。 相似文献
24.
随着人们安全健康意识的提高,食品中农药残留问题更加受到重视。为此,对样品预处理研究进展及农药残留快速检测技术研究进展进行综述,并简单介绍各种方法的优缺点。 相似文献
25.
The quality and safety of agricultural products is the technique focus of the strategy of rural vitaliza⁃tion. Carbamate pesticide residues are seriously threatening the safety of agricultural product and human life and health. Nowadays, the common detection methods are instrument-based for carbamate pesticide residue, which dis⁃ satisfy the request of an on-site rapid, sensitive and simultaneous detection for multiple carbamate pesticide resi⁃ dues. Based on the home-made monoclonal antibodies against carbofuran and carbaryl respectivity, a microarray for rapid and simultaneous detection of multiple carbamate pesticide residues was developed within 30 min. Under the optimized conditions, the limits of detection(LODs)were found to be 0.11 and 0.09 ng/g, while the linear ranges were 0.33-3000 and 0.18-1500 ng/g for carbofuran and carbaryl respectively. By using spiked peanut samples, it recorded recoveries of 88.4%-98.3%, 90.1%-118.8% for carbofuran and carbaryl respectively. The RSD of intraarray were found at 9.0%, 3.5%, while the RSD of inter-array were recorded at 12.3%, 16.3% respectively. The de⁃
tection results of the microarray were highly consistent with that of HPLC-MS/MS. This proposed microarray provid⁃ ed an on-site high-sensitivity, simultaneous and rapid detection of carbofuran and carbaryl, and could be widely used in the fields of agricultural product quality safety, food safety and environmental monitoring. 相似文献
26.
《Communications in Soil Science and Plant Analysis》2012,43(22):2959-2969
The enzyme urease is responsible for the rapid hydrolysis of urea in agroecosystems where more than 50% of the applied nitrogen (N) can be lost via ammonia volatilization. The objectives of the study were to (1) extract urease from corn (Zea mays L.) and soybean (Glycine max L.) and (2) compare the urease activity from soybean and corn residues to Jackbean (Canavalia ensiformis) urease using Fourier transform infrared spectroscopy (FTI-R). Concentrations of urea and sodium bicarbonate ranging from 0 to 200 mM were analyzed with FTI-R to determine the correlation to peak height. Bicarbonate produced the most responsive peaks to concentration at 1,362 cm?1. Urease extracted from soybean residue was active, producing a bicarbonate peak at 1362 cm?1, whereas no urease activity was observed in corn residue. Variation among urease activities in crop residues could suggest a need for more precise nitrogen management in conservation tillage agroecosystems to reduce ammonia volatilization. 相似文献
27.
从浙江省杭州、嘉兴和绍兴等3个地级市采集了4种不同施肥方式下(分别为施用畜禽粪+化肥、商品有机肥+化肥、沼渣+化肥和单施化肥)的蔬菜地表层土壤样品44个,分析了4类8种抗生素(包括四环素类抗生素的土霉素、四环素和金霉素,喹诺酮类抗生素的恩诺沙星,磺胺类抗生素的磺胺嘧啶、磺胺二甲嘧啶和磺胺甲噁唑及大环内脂类抗生素的泰乐菌素)的残留情况,探讨了施肥方式对蔬菜地土壤中抗生素残留的影响。结果表明,蔬菜地土壤中抗生素的检出率和残留含量与施肥方式密切相关。8种检测的抗生素中土霉素的检出率和残留含量明显高于其他种类的抗生素,土霉素的平均含量占8种抗生素总量平均值的67.03%。抗生素的检出率和平均含量由高至低依次为:土霉素磺胺二甲嘧啶恩诺沙星四环素磺胺甲噁唑、泰乐菌素金霉素磺胺嘧啶;四环素类抗生素磺胺类抗生素。土壤中各类抗生素的检出率及含量均为施用畜禽粪的蔬菜地施用商品有机肥的蔬菜地施用沼渣的蔬菜地单施化肥的蔬菜地,施用畜禽粪的蔬菜地土壤中抗生素残留量明显高于其他蔬菜地。试验结果表明,畜禽粪是蔬菜地土壤抗生素的主要来源,商品有机肥和沼渣的施用对蔬菜地土壤中抗生素的残留也有一定的贡献。 相似文献
28.
纤维素超低酸水解产物的分析 总被引:16,自引:2,他引:16
基于木质纤维素类生物质水解为人类提供乙醇等能源、化工产品的重要性,该文以定量滤纸模拟生物质的主要组分-纤维素,以其超低酸水解试验得到的最佳工况下液体产物和固体残渣为研究对象,通过高效液相色谱(HPLC)结合KS-802糖柱对产物质中糖的种类进行了划分,以GC-MS对副产物进行定性,并通过扫描电镜(SEM)及热重和工业分析元素分析对固体残渣作了从表观到内部的研究,发现纤维素超低酸水解主要生成纤维四糖、三糖和二糖等低聚糖和葡萄糖及果糖,反应副产物有糠醛、羟甲基糠醛、乙酰丙酸及一些小分子酮、醛类和酸类极性化合物,水解残渣已完全改变了原始形貌,热裂解活性增强,残留物中碳和灰分含量有较大增加,最后根据分析结果探讨了纤维素超低酸水解的反应途径,为木质纤维素类生物质水解技术的规模化利用打下基础。 相似文献
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30.
The response of soil organic nitrogen (SON) dynamics to climate may partly be deduced from changes in the concentration and origin of the major N constituents in soil, such as amino acids. In this study, we determined the enantiomers of bound amino acids in 18 native grassland soils (0–10 cm) that were sampled along a transect from central Saskatchewan, Canada, to Southern Texas, USA. Mean annual temperature (MAT) ranged from 0.9 to 23.4 °C and mean annual precipitation (MAP) from 300 to 1308 mm. d-alanine and d-glutamic acid served as markers for the bacterial origin of SON. The d-content of lysine, phenylalanine, and aspartic acid indicated an ageing of the respective SON forms. Deuterium labeling was applied to account for hydrolysis-induced racemization reactions. We found that the concentration of the bacterial biomarkers was weakly but significantly parabolically related to MAT, as previously reported for microbial-derived amino sugars. The age markers d-lysine, d-phenylalanine, and d-aspartic acid comprised 2–15% of the respective l-form. The presence of these compounds demonstrated that the structures that contained these d-enantiomers had survived microbial attack, i.e., these hydrolyzable SON forms were conserved in soil despite a living environment. First estimates indicate that the mean residence time of the lysine-containing organic matter forms extend beyond a century. Within this time-scale we did not find that climate significantly affects the degree of ageing of SON constituents in the studied topsoils. 相似文献