电场耦合高效液相色谱柱改善极性芳烃分离的研究

从燃烧的煤和油中排放出来的极性污染物,包含有多种含氮、氧和硫的极性多环芳烃(PAH),这些极性组分比非极性组分常具有更强的致癌和致突变性。目前,正相高效液相色谱(NP-HPLC)常被用来分离分析这类极性组分。 但是,要提高这些极性组分分离的选择性,现大多采用梯度洗脱的方法。也就是改变流动相极性的方法。本文介绍了一种高压电场耦合色谱柱的新方法。这种技术除了具     

饮用水中铝的萃取-高效液相色谱分析

拟定了金属配合物的萃取 -高效液相色谱法。Al与 8-羟基喹啉反应生成的黄色配合物 ,用氯仿萃取 ,在C8烷基键合固定相上 ,以甲醇 -乙酸乙酯 -水 (体积比 4 0 :2 0 :4 0 )为流动相 ,于波长390nm处测定饮用水中总Al的含量 ( 2 0 -70 0 μg/L)。对萃取条件和萃取百分率 ,色谱分离条件进行了研究 ,讨论了测定的灵敏度、选择性和重现性。     

重金属离子-二乙基二硫代氨基甲酸钠螯合体系的HPLC分析方法研究

采用二乙基二硫代氨基甲酸钠(NaDDC)为螯合剂,对Cu(Ⅱ)、Hg(Ⅱ)、Pb(Ⅱ)、Zn(Ⅱ)、Cd(Ⅱ)、Cr(Ⅵ)六种重金属离子进行了螯合萃取分离体系的方法研究,用HPLC方法建立了上述金属离子的最佳分离条件及定性定量分析方法.结果表明,用C18反相柱(5μm,150×4.6mmi.d.)和流动相(V(乙腈):V(甲醇):V(水)=55:15:30)能有效分离上述重金属离子,最低检测限在0.1～1.6ng范围内,线性范围及线性关系满足定量分析要求.     

枇杷核中提取苦杏仁甙的研究

研究了3个枇杷品种的出核率，利用高效液相色谱检测苦杏仁甙的含量，以及从枇杷核中提取苦杏仁甙的工艺。结果表明，3个品种烘干后核的得率存在显著差异，干核的年产量很大，有综合开发利用价值；提取溶剂以乙醇为好，最合理的工艺组合为：在原料中按料液比1：10加入浓度为80％的乙醇，在65℃时回流提取50min。在40℃功率为80W的条件下超声处理25min。合理选择品种是提高苦杏仁甙得率的关键。     

固相萃取-高效液相色谱法测地表水中11种酚类化合物

建立了固相萃取-高效液相色谱法同时测定地表水中11种酚类化合物的方法。水样经过全自动固相萃取仪富集,以HLB柱为萃取柱,乙腈(含1%乙酸)为洗脱剂,用高效液相色谱仪分析定量。该方法在0.5~5.0 mg/L范围内线性良好,相关系数为0.999 6~0.999 9,11种酚类化合物的纯水加标回收率为82.0%~111%,地表水加标回收率为98.5%~116%,精密度为3.58%~4.67%,检出限为1×10-4~5×10-4mg/L,该方法简单实用、准确可靠,可用于地表水中酚类化合物的同时测定。     

基于ZIF-L的微固相萃取技术测定地表水中痕量典型多环芳烃

制备类沸石咪唑酯骨架ZIF-L材料,将其用作微固相萃取吸附剂,处理水中萘、苊、苊烯、芴、菲、蒽、荧蒽、芘等8种痕量典型多环芳烃,再用HPLC测定。试验表明,ZIF-L对上述多环芳烃的萃取效率明显高于商品化萃取材料C 18和多壁碳纳米管。方法在0.100μg/L^200μg/L范围内线性良好,方法检出限为0.02μg/L^0.03μg/L,标准溶液5次测定结果的RSD为4.7%~9.5%,实际水样加标回收率为84.5%~115%。将该方法用于北太湖5个点位水样的测定,测定值为未检出~3.40μg/L。     

Plant steroid hormones produced under Ni stress are involved in the regulation of metal uptake and oxidative stress in Brassica juncea L

Brassinosteroids (BRs) are involved in the amelioration of various biotic and abiotic stresses. With an aim to explore the role of BRs under heavy metal stress, plants of Brassica juncea L. were grown in pots. The plants were subjected to various concentrations of Nickel metal (0.0, 0.2, 0.4 and 0.6 mM) and harvested on 60th day in order to observe the expression of these hormones. The isolated BRs from the leaves of Brassica plants characterized by GC-MS include 24-Epibrassinolide (24-EBL), Castasterone, Dolicholide and Typhasterole. The effect of isolated 24-EBL was studied on Ni metal uptake and antioxidative defense system in 60 d old plants of Brassica. It was observed that 24-EBL significantly increased the activities of stress ameliorating enzymes and lowered the metal uptake in plants. This is the first report in B. juncea L. plants showing the expression of BRs under metal treatments and effect of the isolated 24-EBL on metal uptake and in oxidative stress management.     

HPLC分析甘草中甘草酸和甘草苷含量

研究不同产地、不同生长期的野生与栽培甘草中甘草酸、甘草苷含量的变化,确定其最佳采收期。为了更好地开发利用甘草资源提供理论依据,建立了分析方法,为甘草的现代质量评价体系提供参考数据,扩大甘草药源。采用高效液相色谱测定不同产地、不同生长期野生与栽培甘草中甘草酸、甘草苷的含量。甘草酸在0.4—6μg范围内具有良好的线性关系,r=0.9999,平均回收率(n=3)为101.83%,RSD=0.74%;甘草苷在0.4—6μg范围内具有良好的线性关系,r=0.9998,平均回收率(n=3)为100.50%,RSD=0.22%。该方法确立了甘草的最佳采收期为9月中旬,种植基地的甘草可代替野生甘草使用,为甘草的药用资源和深入开发利用提供了基础依据。该方法简便、精密度高,结果准确可靠。     

Fate of azadirachtin A and related azadirachtoids on tomatoes after greenhouse treatment

The degradation of the main azadirachtoids on tomatoes was studied after greenhouse treatment. These experiments were carried out at 1 and 5× the concentration recommended by the manufacturer. In all experiments the deposition of azadirachtin A (AZA-A) was below the maximum residue level (MRL). Even if at the highest dose, AZA-A half-life time calculated as pseudo first order kinetic was 1.2 days in agreement with the recommended preharvest interval (PHI) of 3 days. Experiments with a model system showed that sunlight photodegradation is the main factor influencing the rate of disappearance of AZA-A after greenhouse treatment while tomato epicuticular waxes doubled the photodegradation rate of AZA-A in a commercial formulation.     

Decay profile and metabolic pathways of quinalphos in water, soil and plants

The widespread occurrence of pesticide residues in different agricultural and food commodities has raised concern among the environmentalists and food chemists. In order to keep a proper track of these materials, studies on their decay profiles in the various segments of ecosystem under varying environmental conditions are needed. In view of this, the metabolites of quinalphos in water and soil under controlled conditions and in plants, namely tomato and radish in field conditions have been analysed and possible pathways suggested. In order to follow the decay of the pesticide, an HPLC procedure has been developed. Studies conducted in water at different temperatures, pH and organic content reveal that the persistence of the pesticide decreases with the increase in all the three variables. In the three different types of soils studied, the effect of pH is more or less apparent on a similar line. On an average a faster decay is observed in the case of plants than in water and soil. The decay profiles in all these cases follow first order kinetics. The metabolites were identified by GC-MS. The investigations reflect that degradation occurs through hydrolysis, S-oxidation, dealkylation and thiono-thiol rearrangement. The pathways seem to be complex and different metabolites were observed with the change in the matrix. Quinalphos oxon, O-ethyl-O-quinoxalin-2-yl phosphoric acid, 2-hydroxy quinoxaline and quinoxaline-2-thiol were observed in all the matrices. Results further indicate that the metabolites, 2-hydroxy quinoxaline and oxon, which are more toxic than parent compound, persist for a longer time.