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Application Of Flow-injection Analysis In The Determination Of Vitamins

Posted on:2006-01-19Degree:MasterType:Thesis
Country:ChinaCandidate:Z P XieFull Text:PDF
GTID:2121360182461447Subject:Analytical Chemistry
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Chemiluminescence(CL) is defined as the emission of light from an electronically excited state species which is produced during the course of a chemical reaction ,and is observed when the electronically excited product or intermediate formed decays to the ground state with a photon emitted. Due to its high sensitivity,wide linear range and simple instrumentation, the chemiluminescence method has been successfully applied in pharmaceutical science, environmental science and life science , and has become one of the most powerful techniques in analytical chemistry.This thesis has studied the analytical methods of determination of Vitamins.We combined the flow injection technology with chemiluminescence. Three new determination methods of VB1 and one new determination methods of VB2 are reported. The methods have been applied to assay the samples and satisfactory results were obtained. It includes five chapters as follows:Chapter 1 ReviewA review of the development of the chemiluminescence theory, the main type of chemiluminescence reaction and the published chemiluminescence methods for determination of Vitamins is given. It describes the general concept and classification of Vitamin,and the great significance of FA in analysis science in 21st centry.Chapter 2 Determination of VB1 by Flow injection Analysis With Chemiluminescence DetectionObjective: To establish a FIA-CL method for the determination of VB1 in pharmaceutical preparation. Methods: It is based on the enhancement effect of VB1 on the CL intensity of luminol-K3Fe(CN)6 system. The VB1 is protected by HCl solution.The flow rate is2.0 mL/min. Injection is operated using a six-way injection valve fitted with a 50- μ L loop. Results: The calibration curve is linear in the range of 1.0×10-71.0×10-6 mmol/mL and 1.0×10-61.0×10-5 mmol/mL respectively with a detection limit of 3.0×10-8 mmol/mL and a sampling rate of 72 times per hour. The relative standard deviation is 2.80% for the determination of 6.0×10-6 mmol/mL VB1 (n=11) . Conclusion: The method is reliable, accurate and very suitable for the determinationChapter 3 HPLC-FI Chemiluminescence Determination with On-line Electrogenerated HypochloriteA flow-injection chemiluminescence method for the determination of VBi based on its inhibition of chemiluminescence from luminol-hypochlorite system is described. The hypochlorite was electrogenerated on-line by constant current electrolysis.Thus,eliminating instability of hypochlorite solution prepared from commercially available sodium hypochlorite . This method has been connected with HPLC which fitted with a d8 column for sepration so as to determine VBj in urine.The calibration curve is linear in the range of 1.0X 10"s1.0X 10"7 mmol/mL and 1.0X 1071.0X 10"6 mmol/mL respectively with a detection limit of 5.0 X 10"9 mmol/mL . The proposed method is reliable, accurate and very suitable for the determination of VBi in pharmaceutical preparations and in human urine.Chapter 4 Disproportionate Chemiluminescence Determination of VBi With Flow InjectionA FIA -CL method for the indirect determination of VBi based on its effect of chemiluminescence from Na2SO3-NaOH-Luminol system with the help of KIO4 is described. The calibration curve is linear in the range of 1.0X 107—1.0X 10'5 mmol/mL with a detection limit of 5.0X10"8 mmol/mL. The method is reliable,accurate and very suitable for the determinationChapter 5 Determination of VB2 by Flow Injection Analysis with Chemiluminescence DetectionA new chemiluminescence (CL) system for the determination of VB2 has been established. By the fast reduction reaction between chromeum VI and VB2,chromeum III was generated to react with luminol and hydrogen peroxide in alkaline aqueous solution and hydrogen peroxide to produce CL. The CL emission intensity was correlated with VB2 concentration in the range 1.0X 10"10—1.0X 10"9 mmol/mL , 1.0X 10"91.0X 10"8 mmol/mL, 1.0X 10"81.0X 10'7 mmol/mL, 1.0X 10"71.0X 10"6 mmol/mL, 1.0X 10"61.0X 10° mmol/mL respectly,and the detection limit was 3.0X10"" mmol/mL VB2. The relative standard deviation is 1.8 % for the determination of 6.0 X 109 mmol/mLVB2(n=9) .The average recovery is 101.3%. The method is reliable, accurate and very suitable for the determination of VB2.
Keywords/Search Tags:flow injection, chemiluminescence, VB1, VB2
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