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Study On The High Performance Liquid Chromatography And Pretreatment Technology Applied To Pharmaceutical And Environmental Analysis

Posted on:2010-04-22Degree:MasterType:Thesis
Country:ChinaCandidate:J H SunFull Text:PDF
GTID:2121360275451901Subject:Analytical Chemistry
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High performance liquid chromatography(HPLC) as an important modern measurement and separation means now is one of high efficient and rapid analysis and separation technology emerging in the 1970's.Due to its characteristics of convenience,high rapidness,sensitivity and fairly accuracy,it has been widely used in the areas of production of medicine,foodstuff,and environment etc.This paper includes two sections-review and research report.In the review section,the HPLC and pretreatment technologies and their present application in the drug and environmental samples are summarized.In the next research report section,which is composed of components as follows: 1) Determination of caffeic acid and ferulic acid in oral liquid by RP-HPLC;2) Cloud point extraction for the determination of carbaryl and fenobucarb in water samples by high performance liquid chromatographic detection;3) Determination of phthalate esters in environmental water samples by temperature-controlled ionic liquid dispersive liquid-phase microextraction;4) Determination of carbaryl in vegetables with carbon nanotubes dispersive solid phase extraction and HPLC detection.1.Determination of Caffeic Acid and Ferulic Acid in Oral Liquid by RP-HPLCA HPLC method was established for the determination of ferulic acid and caffeic acid in oral liquid.Shim-pack VP-ODS column(150×4.6 mm,3μm) was used with a mobile phase of acetonitrile - 3%acetic acid(11:89 by volume).The flow rate was 1.0 mL/min and the contents of ferulic acid and caffeic acid were detected at wavelength of 321 nm.The calibration curve was linear in the range of 0.126~63.0μg/mL(r = 0.9997) for caffeic acid and 0.120~24.0μg/mL(r = 0.9999) for ferulic acid.The detection limit was 42 ng/mL for caffeic acid and 43 ng/mL for ferulic acid.The average recovery was 100.7%with RSD 2.11%for caffeic acid and was 99.9%with RSD 2.12%for ferulic acid.The average content of the sample was 3.26μg/mL for caffeic acid and 2.36μg/mL for ferulic acid. 2.Cloud Point Extraction for the Determination of Carbaryl and Fenobucarb in Water Samples by High Performance Liquid Chromatographic DetectionThe feasibility of employing cloud point extraction(CPE) as the extraction and preconcentration method for the recovery of carbaryl and fenobucarb from water samples followed by HPLC-UV analysis was demonstrated.The surfactant Triton X-100 was used to extract and preconcentrate the analytes.The optimum conditions of CPE were as follows:10%(w/v) Triton X-100,10%(w/v) sodium sulfate,equilitration temperature 50℃,equilitration thne 45 min;chromatographic conditions:mobile phase of methanol-water with 55:45(V/V ),Shim-pack VP-ODS column(150×4.6 mm,3μm),flow rate of 1.0 mL/min,the run time of 25 min;the detection wavelength was 220 nm in the frist 10 min and 200 nm in the last 15 min.The results showed that the linear ranges of detection were 2~1000μg/L for carbaryl with the correlation coefficient of 0.9995 and 60~10000μg/L for fenobucarb with the correlation coefficientof 0.9990.The average recoveries for the water samples were 94.49%~96,1%for carbaryl and 92.2%~101.7%for fenobucarb.3.Determination of Phthalate Esters in Environmental Water Samples by Temperature-Controlled Ionic Liquid Dispersive Liquid-Phase MicroextractionA simple,fast and efficient sample preparation approach,temperature-controlled ionic liquid (IL) dispersive liquid-phase microextraction,coupled with high-performance liquid chromatography and UV detection has been developed for the extraction,preconcentration and determination of phthalate esters in water samples.The influences of some important parameters such as the kind and volume of extraction IL,extraction time,extraction temperature,centrifugation time,and salt effect on the extraction efficiency were investigated.Under the optimum extraction conditions including 40μL of 1-octyl-3-methylimidazolium hexafluorophosphate([C8MIM][PF6]) as the extraction IL, extraction time of 20 min,extraction temperature of 60℃,centrifugation time of 10 min and without salt addition,the model analytes diethyl phthalate(DEP),dibutyl phthalate(DBP),and dioctyl phthalate(DOP) exhibited good linear relationship in the concentration range of 0.005~10.0 mg/L for DEP and 0.005~50.0 mg/L for DBP and DOP with the correlation coefficient of 0.9988 for DEP,0.9994 for DBP and 0.9991 for DOP,respectively.The detection limits(S/N = 3) were 0.0027 mg/L for DEP,0.0022 mg/L for DBP and 0.0007 mg/L for DOP.The relative standard deviations for the extraction of 5.0 mg/L DEP,DBP and DOP were 2.5%,5.3%,and 4.0%(n = 6),respectively. The recoveries of phthalate esters from tap and river water samples were in the range of 87.2%~103.8%.This method can be successfully applied for the determination of phthalate esters in environmental water samples.4.Determination of Carbaryl in Vegetable Samples with Carbon Nanotubes Dispersive Solid Phase Extraction and HPLC detectionA new method for the determination of carbaryl in vegetable samples was established with carbon nanotubes dispersive solid- phase extraction and HPLC-UV detection.Under the optimized instrumental conditions,the detection limit of carbaryl was 22μg/kg.A good linear relationship was obtained between the concentration 0.1~10μg/mL and peak area with the correlation coefficient of 0.9980.The average recoveries of carbaryl spiked in vegetable samples ranged from 81.3%to 105.1%with the relative standard deviations ranging from 1.7%to 6.9%.The carbon nanotubes dispersive Solid- phase extraction method has the advantages of simplicity,less matrix interferences, good accuracy and reproducibility.
Keywords/Search Tags:High-performance liquid chromatography, Pharmaceutical analysis, Environmental analysis, Cloud point extraction, Dispersive liquid-phase microextraction, Dispersive solid phase extraction
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