固相萃取-反相高效液相色谱法测定环境水体中卡马西平

建立了固相萃取-反相高效液相色谱法测定水中痕量卡马西平的方法.以C18固相萃取柱对水样固相萃取,再经Agilent ZORBAX Exlipse XDB-C18色谱柱分离,在紫外检测器上检测.考察了洗脱液、流动相比例的影响.确定洗脱液选用甲醇(17+3)溶液,流动相选择甲醇(11+9)溶液.结果线性关系良好(在0.2～...     

固相萃取-超高效液相色谱-电喷雾串联质谱法检测梨树叶中熊果苷

建立了固相萃取净化、超高效液相色谱-串联质谱检测梨树叶中熊果苷含量的方法.将粉碎的梨树叶样品用甲醇提取,ENVITM-18固相萃取柱净化,超高效液相-电喷雾串联四级杆质谱检测,外标法定量.测定时用 Acquity UPLC HSS T3 色谱柱(50 mm×2.1 mm,1.8μm)分离,甲醇-水(V/V,7+93)洗...     

固相萃取-高效液相色谱法测定枸杞中的类胡萝卜素

研究了固相萃取富集和预分离,高效液相色谱测定枸杞中的类胡萝卜素的方法;枸杞中的类胡萝卜素用WatersXterraTMRP18固相萃取小柱预分离,以WatersXterraTMRP18(3.9×150mm,5μm)液相色谱柱为固定相,甲醇 四氢呋喃(4 1)为流动相分离,用二极管矩阵检测器检测,检测波长为450nm。方法标准回收率为95%～103%。用该方法测定了几种枸杞样品中的类胡萝卜素。     

高效液相色谱法快速测定三白草中黄酮类物质

研究了用固相萃取预分离,高效液相色谱法测定三白草中黄酮类物质。三白草中的黄酮用甲醇(90 10)加热回流提取,提取液用Waters Sep-Pak-C18固相萃取小柱预分离,以ZORBAXStable Bound(4.6 mm×50 mm,1.8μm)色谱柱为固定相,磷酸(2 998)和甲醇(以体积比50比50)为流动相,在该色谱条件下,三白草中主要的黄酮成分在1.5 min内可达到基线分离;用紫外二极管矩阵检测器检测。用该方法测定了5种三白草样品中的黄酮类物质,回收率在97%~103%之间,相对标准偏差在1.6%~2.2%之间。     

固相萃取富集-高效液相色谱法测定环境水中多菌灵和噻菌灵

建立了以固相萃取技术富集，高效液相色谱法进行分离和检测多菌灵和噻菌灵2种杀菌剂的方法。环境水中的多菌灵和噻菌灵用3M Empore 6mL C18 Cartridge进行固相萃取。以Hypersil ODS柱为分析柱，优化得到高效液相色谱分离条件：流动相为甲醇-水(50：50，V/V)；流速为0．7mL／min；柱温为55℃；在286nm波长下检测，检出限为0．05mg／L。本法操作简便，灵敏，回收率高。     

固相萃取富集-高效液相色谱分离和测定邻甲苯胺和邻硝基甲苯

建立了以固相萃取技术进行富集 ,高效液相色谱进行分离和检测邻甲苯胺和邻硝基甲苯的方法。污染水中的邻甲苯胺和邻硝基甲苯采用Sep pakC1 8萃取柱进行固相萃取。色谱分离条件是 :Shim PackCLCODS(1 5 0mm× 4 .6mmid ,5 μm)柱为分析柱 ,甲醇 水 =60∶4 0 (V V)为流动相 ,流速为 1 .0mL min,邻甲苯胺和邻硝基甲苯的紫外检测波长分别为 2 3 0nm和 2 5 4nm ,本法具有良好的灵敏度和重现性。     

固相萃取富集高效液相色谱法测定苯氧乙酸和2,4-二氯苯氧乙酸

建立了以固相萃取技术进行富集 ,高效液相色谱法进行分离和检测苯氧乙酸和 2 ,4 二氯苯氧乙酸的方法。环境水中的苯氧乙酸和 2 ,4 二氯苯氧乙酸用Sep PakC18Cartridge进行固相萃取。液相色谱的条件是 :Shim PackCLCODS柱为分析柱 ;甲醇 水 (9∶1,V/V)为流动相 ;流速为 1mL/min ;在UV 2 75nm波长下进行检测。本法具有良好的灵敏度和重现性     

高效液相色谱法快速测定满山红中槲皮素和杜鹃素的研究

研究了用固相萃取预分离,高效液相色谱法测定满山红中槲皮素和杜鹃素。槲皮素和杜鹃素用90%甲醇加热回流提取,提取液用Waters Sep-Pak-C18固相萃取小柱预分离,然后用ZORBAX Stable Bound(50×4.6 mm i.d.,1.8μm)色谱柱,以0.2%的磷酸和甲醇(52∶48,V/V)为流动相,槲皮素和杜鹃素在1.0 min内可达到基线分离;用紫外二极管矩阵检测器检测。方法的加入标准回收率为98%~102%,相对标准偏差为1.6%~1.8%。本法可用于满山红样品中的槲皮素和杜鹃素的测定,结果满意。     

分子印迹在线固相萃取分离奥克托今合成反应中间体

采用分子印迹在线固相萃取和液相色谱-质谱联用技术建立了奥克托今合成反应中间体1,3,5,7-四乙酰基-1,3,5,7-四氮杂环辛烷(TAT)与1,3,5-三乙酰基-1,3,5-三氮杂环己烷(TRAT)的分离鉴定方法。固相萃取填料采用TAT分子印迹聚合物,液相色谱分离检测采用亲水色谱柱。首先以乙腈为固相萃取柱上样溶剂,流速为0.1 mL/min,然后以乙酸乙酯淋洗萃取柱,用甲醇洗脱,并以甲醇为流动相对洗脱溶液进行液相色谱分离,与质谱仪联用鉴定各分离组分。在上述条件下,TAT回收率在79％~93％,检出限为1.8 mg/L (3σ),线性范围为6.0~500.0 mg/L,富集倍数400倍。     

固相萃取高效液相色谱法测定蜂王浆啤酒中的1O-羟基-2-癸烯酸

建立了固相萃取高效液相色谱法测定蜂王浆啤酒中10-羟基-2-癸烯酸含量的方法。采用固相萃取技术富集蜂王浆中的10-羟基-2-癸烯酸,以甲醇-水-磷酸(体积比为50：50：0．5)为流动相,ODS柱分离,用紫外检测器于215nm处检测。10-羟基-2-癸烯酸的浓度在0．5-100．0μg/mL范围内与其色谱峰峰面积呈良好线性关系(r=0．9999),回收率为98％-108％,RSD为2.1％。     

Parathion und Malathion

Ohne Zusammenfassung     

Micellar Effects on Hydrolysis of Parathion

Kinetics of the reaction between a pesticide (Parathion) and α-nucleophile hydroxamate ion (N-methyl 4-chlorobenzohydroxamate ion and N-methyl 4-chlorothiobenzohydroxamate ion) have been studied in the presence of various novel cationic surfactants at 27°C. The reaction exhibits pseudo first order kinetics and the rate of hydrolysis increased with surfactant concentration.     

Zur Bestimmung von Parathion in Tomaten

Ohne Zusammenfassung     

Methyl Parathion Degrading Enzyme‐based Nano‐hybrid Biosensor for Enhanced Methyl Parathion Recognition

Enzyme‐based electrochemical biosensors with sufficient sensing specificity are useful analytical tools for detection of biologically important substances in complicated systems. Here, we present the design of a nano‐hybrid biosensor for the specific and sensitive detection of methyl parathion (MP). The nano‐hybrid sensing film was prepared via the formation of Au nanoparticals (AuNPs) on silica nanoparticles (SiNPs), mixing with multiwall carbon nanotube (MWNTs) and subsequent immobilization of methyl parathion degrading enzyme (MPD). The fabrication procedure was characterized by scanning electron images, linear scan voltammetry and electrochemical impedance spectroscopy. The combined MPD exhibited high affinity to it substrate and thus a selective, sensitive, fast and cheap method for determination of MP, quantitatively was proposed. A significant synergistic effect of nano‐hybrid on the biosensor performance was observed in biosensing MP. The square wave voltammetric responses displayed well defined peaks, linearly proportional to the concentration of MP in the range from 0.001 to 5.0 μg/mL with a detection limit of 0.3 ng/mL. The proposed biosensor also showed good precision and reproducibility, acceptable stability and accuracy in garlic samples analysis. It provided a platform for the simple and fast construction of biosensors with good performance for the determination of enzyme‐specific electroactive species.     

On the Utilization of Boron Doped Diamond Electrode as a Sensor for Parathion and as an Anode for Electrochemical Combustion Of Parathion

This work proposes the utilization of a boron doped diamond (BDD) electrode as a sensor for pesticides and as well as an anode for electrochemical combustion of Parathion in spiked, pure and natural waters. The square‐wave voltammetry was selected as the electroanalytical technique and the Britton–Robinson buffer as the electrolyte. The electrochemical reduction responses of Parathion were analyzed and compared with those previously obtained using a hanging mercury electrode (HMDE). The detection and quantification limits were calculated from the analytical curves both for BDD and HMDE in Milli‐Q water (2.4 and 7.9 μg L^?1 and 3.9 and 12.8 μg L^?1 respectively) showing only a slight improvement when used BDD. However, if the application involves polluted natural waters the improvement is accentuated due to the very low adsorption characteristics of BDD, which prevent the fouling of electrode surface by organic pollutants. The BDD was also used as anode for electrochemical remediation of Parathion contamination. In this case, electrolysis was carried out in high positive potential (3.0 V) and lead the electrochemical combustion of Parathion to CO₂ and H₂O, as measured by the diminishing of total organic carbon in the electrolyte.     

对硫磷分子烙印传感器的制备及应用

对硫磷分子烙印传感器的制备及应用;分子烙印传感器;对硫磷;纳米TiO2;微分脉冲伏安法;液相沉积     

Colorlmetric Analysis of Malathion and Parathion Using Fluoboric Acid

Abstract

Monohydroxyfluoboric acid is described as a reagent for the determination of the organophosphorus compounds malathion and parathion. The reagent breaks the ether linkage to phosphorous to form a phosphoro-or phosphono-fluoridate which is then coloriraetrically determined by reaction with hydrogen peroxide and 2,7-diaroinofluorene. From 0.01 to 0.50 mg./ml. of the organophosphorus compounds can be determined.     

对硫磷化学发光酶联免疫吸附分析方法的建立和评价

建立了基于多克隆抗体的对硫磷间接竞争化学发光酶联免疫吸附分析方法(icCLEIA)。以三氯硫磷为原料,经三步取代反应合成对硫磷半抗原,通过活泼酯法将半抗原分别与牛血清蛋白(BSA)和卵清蛋白(OVA)偶联,制备免疫抗原和包被抗原。经免疫新西兰大白兔,获得对硫磷抗血清。通过优化条件参数,建立了对硫磷的icCLEIA分析方法。本方法的检测线性范围为0.24～15.83!g/L;半抑制浓度IC50为1.14!g/L;检出限为0.09!g/L;对蔬菜样品和水样品的平均添加回收率为74.6%～121.0%。本方法可用于实际样品中痕量对硫磷残留检测。     

荧光光度法测定环境水中微量甲基对硫磷

研究了荧光分光光度法测定环境水中甲基对硫磷的一。在吲哚丙酮溶液０．２５％，过硼酸钠溶液０．２５％溶液中，温度５℃、λｅｘ／λｅｍ＝４１０ｎｍ／４９０ｎｍ，检出限５．０（５．２）μｇ／Ｌ，线性范围０－２．０（２．６）ｍｇ／Ｌ，回收率达９８－１０２％，结果满意。     

Die ma?analytische Bestimmung von Parathion mit Chloramin T

Ohne Zusammenfassung