| Flow injection fluorescence spectrometry has the advantages of fluorescence spectrometry and flow injection technique. It has been widely used in the determination of pharmaceutical. Most pharmaceutical molecules only have weak fluorescence substance itself or not, they all need to enhance fluorescence intensity with some reactions. In this paper, we make these pharmaceuticals to produce the strong fluorescent substances through oxidation-reduction reaction. However, some products of the fluorescence intensity were instability, the conditions were not easily controlled in the steady-state. Based on this, combined with flow injection analysis and time scanning technology, a new fluorescence spectrometry for the determination of pharmaceuticals: phenoxymenylpenicillin potassium, carbamazepine, chlopromazine hydrochloride, perphenazine, promethazine hydrochloride, dioxopromethaine hydrochloride, famciclovir and enoxacin. The proposed method has the advantages of simplicity, rapidity, precision and sensitivity. It has been successfully applied to the determination of these pharmaceuticals in tablets, capsules, injections, human urines and serums with satisfactory results.There are three chapters in this thesis.Chapter one: Flow injection fluorophotometric method in the pharmaceutical research progressIn the part, the flow injection fluorophotometric methods for pharmaceutical analysis were summarized in detail about the literature at home and abroad over the past decade.Chapter two: Application of time scanning fluorescence spectrometry in the pharmaceuticals by flow injection analysis with on-line oxidizing1. A time scanning fluorophotometric method for the determination of phenoxymenyl penicillin potassium by flow injection analysisPhenoxymenylpenicillin potassium is a weak fluorescent substance and can react with sulfuric acid to produce stronger fluorescent species in the buffer solution pH=5.72 britton-robinson. Based on this, combined with flow injection analysis and time scanning technology, a new fluorimetric method for the determination of phenoxymenyl penicillin potassium by the oxidation of sulfuric acid is proposed. The experimental conditions that influence the fluorescence intensity were investigated and optimized. The excitation and emission wavelengths are 236.0nm and 306.0nm, respectively. The linear range is 3.6×10-5 g/L~4.0×10-2 g/L with the detection limit of 1.0×10-5 g/L. The relative standard derivation is 0.6% (n=11, c=1.0×10-3g/L), The frequency of sample introduction is 78 samples per hour. The method has been used for the determination of phenoxymenyl penicillin potassium in tablets and human urines with satisfactory results.2. A time scanning fluorescence spectrometry for the determination of carbamazepine by flow injection analysisCombined with flow injection analysis and time scanning technology, a new fluorophotomeric method for the determination of carbamazepine was proposed. The method was based on the reaction between carbamazepine and potassium permanganate in the medium of sulfuric acid, the fluorescence intensity enhanced significantly. The excitation and emission wavelengths are 357.0nm and 480.0nm, respectively. The experimental conditions that influence the fluorescence intensity were investigated and optimized. The linear range was 0.0012μg/mL~1.2μg/mL, the detection limit was 5.2×10-5μg/mL, the relative standard derivation was 0.5% (n=5, c=0.1μg/mL), The frequency of sample introduction is 90 samples per hour. The method has been applied to the determination of carbamazepine in tablets, human urines and serums with satisfactory results.3. Flow injection on-line oxidizing fluorophotometric method for the determination of phenothiazinesA novel fluorescent system coupled with flow injection technique was developed for the determination of three phenothiazine drugs, namely, chlopromazine hydrochloride, perphenazine and promethazine hydrochloride. The experiments indicated that the fluorescence signal of three drugs was weak. The fluorescence intensity can be sensitized strongly by the reaction with oxidation. Some oxidizing agents including H2O2, K2Cr2O7, KClO3, KIO4, Ce(Ⅳ), Mn4+ and KMnO4 were studied respectively. The results showed that the reaction between the three drugs and KMnO4 is the best among above oxidants. But the the fluorescence intensity of oxidation products were instability, the experimental conditions were not easily controlled in the steady-state. Flow-injection analysis (FIA) has many analytical advantages, so the sample can be determined in non-steady state. On this basis, combined with flow injection analysis and time scanning technology, a new on-line oxidizing fluorescent method was established for the determination of the three phenothiazine drugs. The experimental conditions that influence the fluorescence intensity,such as: the reaction medium and pH, the type of oxidant, the influence of surfantants and earth ions, the flow rates, the length of mixing tube, et al were investigated and optimized. Under optimal experimental conditions, the fluorescence of the system were measured atλex =312nm andλem=436nm for cholorpromazine hydrochloride,λex =309nm andλem=386nm for perphenazine,λex=304nm andλem =380nm for promethazine hydrochloride. The linear ranges of the method were 0.12~36μg/mL for cholorpromazine hydrochloride, 0.4~20μg/mL for perphenazine and 0.4~36μg/mL for promethazine hydrochloride. The detection limits were 3.6ng/mL, 0.02μg/mL and 0.03μg/mL, respectively. The frequency of sample introduction were 90, 106 and 128 samples/h, respectively. The proposed method has the advantages of simplicity, rapidity, precision and sensitivity. It has been successfully applied to the determination of phenothiazines in tablets and human urines with satisfactory results.4. A time scanning fluorophotometric method for the determination of dioxopromethaine hydrochloride by flow injection analysis Dioxopromethaine hydrochloride can react with sulfuric acid to produce stronger fluorescent species. Based on it, combined with flow injection analysis and time scanning technology, a new flow-injection fluorescence method for on-line determination of dioxopromethaine hydrochloride is established. The experimental conditions that influence the fluorescence intensity were investigated and optimized. The excitation and emission wavelengths are 274.0nm and 376.0nm, respectively. The linear range is 2.8×10-4g/L~4.0×10-2g/L, the detection limit is 1.1×10-5g/L, the relative standard derivation is 0.5% (n=11, c=1.2×10-3g/L), the frequency of sample introduction is 100 samples/h. The method has been used for the determination of dioxopromethaine hydrochloride in different tablets, human urines with satisfactory results.Chapter three: Application of a micellar enhanced-sensitive and direct fluorescence spectrometry in the pharmaceuticals by flow injection analysis1 A time scanning fluorescence spectrometry for the determination of famciclovir by flow injection analysisFamciclovir is a strong fluorescent substance. Based on it, combined with flow injection analysis and time scanning technology, a new flow-injection fluorescence method for the determination of famciclovir is established. The experimental conditions that influence the fluorescence intensity were investigated and optimized. The excitation and emission wavelengths are 309.0nm and 380.0nm, respectively. The linear range is 2.8×10-4g/L~4.0×10-2g/L, the detection limit is 5.8×10-6g/L, the relative standard derivation is 0.4% (n=11, c=4.0×10-4g/L), the frequency of sample introduction is 100 samples/h. The method has been used for the determination of famciclovir in different tablets, capsules, human urines with satisfactory results.2 A micellar enhanced-sensitive fluorescence spectrometry for the determination of enoxacin by flow injection analysisThe fluorescence characteristics of enoxacin-aluminum(III) in micellar system was studied. The experiment indicateded that in the buffer solution of (CH2)N6-HCl medium with pH 5.80, the surface active agent of sodium dodecyl sulfate(SDS) could improve the fluorescence intensity of enoxacin-aluminum(III) remarkably. Based on this, combined with flow injection analysis and time scanning technology, a new fluorophotometric method for the determination of enoxacin was developed. The experimental conditions that influence the fluorescence intensity were investigated and optimized. The maximum excitation wavelength is 267.0nm, while the maximum emission wavelength is 400.0nm. Under optimal experimental conditions, the linear range was 0.002 mg/L~0.8 mg/L, the detection limit was 1.7μg/L (3σ). The recovery was in the range of 97.8%～100.4%. The frequency of sample introduction is 90 samples per hour. The method is simple, rapid and sensitive, and has been used for the determination of enoxacin in tablets, capsules and injections with satisfactory results.
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