橘园土壤中嘧菌酯的残留消解动态分析

为了了解嘧菌酯在柑橘园土壤中的消解动态规律,采用气相色谱-电子捕获检测法,对贵州、湖南、浙江3地的橘园土壤中嘧菌酯残留进行了检测,并建立了嘧菌酯在土壤样品中的残留检测体系.结果表明,在试验检测条件下,嘧菌酯的最小检出量为1×10-11 g,相对保留时间为4.86 min;添加回收率为98.3％～105.4％,变异系数为5.0％～7.2％,标准偏差为5.15％～7.15％,均能达到我国农药残留检测的要求;湖南、浙江、贵州柑橘园土壤中嘧菌酯的消解半衰期分别为14.0、13.2、11.6d.这表明在自然条件下,嘧菌酯在土壤中消解较快,不会造成土壤中累积性残留污染.     

香稻香气特征化合物2–乙酰基–1–吡咯啉测定方法的建立

建立了一种利用顶空固相微萃取–气相色谱法(HS–SPME–GC)检测香稻香味特征化合物2–乙酰基–1–吡咯啉(2–acetyl–1–Pyrroline,2–AP)的方法。在合成2–AP标准物质的基础上,通过正交试验得到最佳萃取条件为萃取温度60℃、萃取时间45 min。在最佳萃取条件下,该检测方法的线性范围为0.5~4.0μg/g,相对标准偏差≤8.54%,回收率为96.3%~103.5%,检出限为0.045 5μg/g,定量限为0.152μg/g。利用该方法测定6种不同香稻大米2–AP的含量,结果表明,该方法能有效地检测香米的2–AP含量。     

高效液相色谱法测定青贮饲料桑中的乳酸、乙酸和丙酸含量条件探讨

本文应用高效液相色谱法(HPLC)对青贮饲料桑中的乳酸、乙酸和丙酸含量测定进行了研究.通过对色谱柱、流动相、流速及样品处理条件进行优化,建立了一种应用HPLC法同时测定青贮饲料桑中乳酸、乙酸和丙酸含量的方法.研究结果表明:乳酸、乙酸和丙酸在一定浓度下具有良好的线性关系,且相关系数R2均大于0.999,加标回收率为98....     

潮州6种蔬菜汤中F~-·Cl~-·NO_2~-·NO_3~-的同时测定

[目的]同时测定潮州蔬菜汤中F-、Cl-、NO2-和NO3-的含量。[方法]利用WICⅡ-型离子色谱仪,测定潮州不同鲜度6种蔬菜汤中F-、Cl-、NO2-和NO3-的的含量。[结果]菜汤中NO3-的含量较高;菜汤中有适宜的F-、Cl-含量。[结论]保鲜处理放置的蔬菜中,NO2-、NO3-含量增加。     

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。     

DETERMINATION OF METALLIC IRON IN HIGH TITANIUM SLAG BY HEADSPACE GAS CHROMATNGRALHY

The following details are discussed in the present paper, after high titanium slag and H3PO4 is put in the closed system,the .reaction takes place under controlled temperature conditions, and the gas produced is collected. The two phases of gas liquid attain kinetic equilibrium, ihe gas above the liquid is used to make GC analysis with the aid of chromatographic column of 5A molecular sieve, TCD and N2 30ml/min. Satisfactory quantitative results can be achieved with simple instruments and uncomplicated operation technique.     

印度Leh地区沙棘籽油中脂肪酸测定

本文分析了印度Leh地区沙棘籽油中脂肪酸各成分的含量,结果显示沙棘种子含油量为17.61%,籽油富含油酸(23.012%)和亚油酸(30.162%).     

一种利用气相色谱快速检测瘤胃体外发酵液中三甲胺浓度的方法

本试验旨在建立一种利用气相色谱快速检测瘤胃体外发酵液中三甲胺浓度的方法.瘤胃体外发酵试验设置2个组,对照组(n=4)和试验组(n=4),试验组每个发酵瓶中添加0.0414 g三甲胺盐酸盐,发酵24 h.采用10 mol/L氢氧化钾溶液对发酵液样品进行预处理,使用WEL-PEG20M色谱柱和氢火焰离子检测器对三甲胺进行分...     

Characterization of humus-protease complexes extracted from soil

Pyrophosphate (140 mM, pH 7.1) extracts of two arable soils and one pasture soil were ultrafiltrated separating the extracted material into three fractions: A_I with nominal molecular weight (nmw) > 100 kD, A_II with nmw between 10 kD and 100 kD and R with nmw < 10 kD. Protease activity was determined in the fractions by using three different substrates: N-benzoyl-l-argininamide (BAA), specific for trypsin; N-benzyloxy-carbonyl-l-phenylalanyl l-leucine (ZPL), specific for carboxypeptidases; and casein, essentially a non-specific substrate. The derivative fractions were also analysed for their amino acid N and humic (HA) and fulvic (FA) acid contents. The organic matter of extracts and derivative fractions obtained from the pasture soil was analysed by isoelectric focusing (IEF) and that of fractions analysed by pyrolysis gas chromatography (Py-GC). Activities of the extract were monitored for their thermal stability and those of the extract and derivative fractions for their optimal pH.Due to the mechanical disintegrating action of sodium pyrophosphate over the humic substances during the fractionation process the amount of total organic C and FA in the fractions was ranked as R > A_II > A_I. The lowest amino acid N/organic C was found in the R fraction, whereas A_II fraction was rich in humic acids, carbohydrates and amino acid N and A_I fraction showed the lowest carbohydrate content. At least 70% of the total BAA- and ZPL-hydrolysing activity was associated to particles with nmw higher than 10 kD and at least 30% of these activities were present in particles with nmw higher 100 kD. Casein-hydrolysing activity was quite evenly distributed among the three fractions (A_I, A_II and R). The extracted protease-organic complexes were resistant to thermal denaturation and some of them showed optimal activity at pH values higher than 10 as a result of the polyanionic characteristics of the humic material surrounding enzyme molecules and of the presence of alkaline protease. Comparison of data obtained in Py-GC analyses and in protease activity suggests that BAA-hydrolysing activity was associated to a highly condensed humic matter and ZPL-hydrolysing activity to less resistant humic substances, while at least some of the extracted casein-hydrolysing activity was present as glyco-proteins not associated to humus. BAA-hydrolysing activity was probably inhibited by fresh organic matter of carbohydrate origin whereas lignin derived organic matter probably inhibited ZPL- and casein-hydrolysing activity.