| Famotidine and thiadiazide in the medicinal properties, have unique position. New RRS, SOS and FDS methods for the determination of famotidine (FMTD), chlorpromazine hydrochloride (CPZ) and promethazine hydrochloride (PMZ) have been established and developed. It can be used in the determination of trace drugs in the pharmaceutical preparation and food. Main investigated systems are listed as follow:1. Study on the ternary ion-association complex nanoparticles of palladium(Ⅱ)-famotidine and halogen-fluorescein dyes by the resonance Rayleigh scattering and resonance nonlinear scattering spectra and their applicationIn pH 3.5-4.7 NaAc-HAc buffer medium, famotidine (FMTD) reacted with palladium (Ⅱ) (Pd (Ⅱ)) to form chelate cation, which further reacted with halogen-fluorescein dyes (HF) such as dichlorofluorescein (DCF), dibromofluorescein (DBF), diiodofluorescein (DIF), erythrosine (ER), eosine (EY) and eosin (EE) to form ternary ion-association complex [Pd(FMTD)]·(HF)2. The Pd(FMTD)·(HF)2 further aggregate to form average diameter of about 9 nm nanoparticles by hydrophobic forces and Van der Waals forces. As a result, the absorption bands of DCF, DBF, DIF, ER, EY, EE were shifted, the fluorescences of them were quenched and the resonance Rayleigh scattering (RRS), second-order scattering (SOS) and frequency doubling scattering (FDS) were enhanced greatly. The maximum absorption wavelengths of [Pd(FMTD)·(HF)2] were located at 476 nm (DCF system),540 nm (DBF system),553 nm (DIF system),560 nm (ER system),547 nm (EY system),549 nm (EE system) and the maximum RRS, SOS and FDS wavelengths of those were located at 302～361 nm, 536～564 nm and 320～390 nm, respectively. The three△I were proportional to the FMTD concentration in a certain range and the detection limits were 1.0～2.6 ng/mL (RRS method),4.2～13.0 ng/mL (SOS method) and 3.6～10.7 ng/mL (FDS method), respectively. Based on it, a high sensitive, good selective, rapid and new molecular spectrum method had been proposed to determine FMTD. It can be applied to determine FMTD in pharmaceutical preparation such as tablets, gelatin capsule and injection. In this work, the optimum reaction conditions, the influences of coexisting substances and the properties of analytical chemistry are investigated, and the mechanism of ion-association reaction and the reasons of enhancement for RRS are also discussed by the change of UV, F and the formation of nanoparticles.2. Study on the ternary mixed ligand complex of Hg(Ⅱ)-famotidine and anionic surfactant by the resonance Rayleigh scattering, second-order scattering and frequency doubling scattering spectra and their analytical applicationsIn pH 5.9 NaAc-HAc buffer medium, FMTD reacted with Hg(Ⅱ) to form chelate cation ([Hg(FMTD)]2+), which further reacted with anionic surfactants (AS) such as sodium dodecylsulfate (SLS), sodium dodecylbenzene sulfonate (SDBS) and sodium dodecylsulphate (SDS) to form ternary mixed ligand complex ([Hg(FMTD)(AS)2]). As a result, RRS, SOS and FDS were enhanced greatly. Their maximum wavelengths were located at 345～352 nm,544 nm and 352 nm, respectively. The three scattering intensity (△I) were proportional to the FMTD concentration in a certain range, and their detection limits were 3.3～3.9 ng/mL (RRS method),14.6～16.3 ng/mL (SOS method) and 7.0～8.5 ng/mL (FDS method). Based on it, the simple, rapid, accurate and sensitive light scattering methods had been proposed to determine FMTD in injection, serum and urine sample. The effects of formation of [Hg(FMTD)(AS)2] on absorption and RRS spectra were investigated, and the reasons of enhancement for RRS were also discussed.3. Study on the interaction between palladium(Ⅱ)-famotidine and halogen-fluorescein dyes by fluorescence quenching method and their analytical applicationsThe interaction between palladium(Ⅱ)-famotidine and halogen-fluorescein dyes (HF) was investigated by fluorescence and absorption spectrum. In pH 3.2～4.1 NaAc-HAc buffer medium, FMTD reacted with palladium(Ⅱ) (Pd(Ⅱ)) to form chelate cation, which further reacted with dibromofluorescein (DBF), eosine (EY), eosin (EE) and tetrabromotetrachloroflurescein (TCBF) to form ternary ion-association complexes [Pd(FMTD)]·(HF)2. As a result, the absorption bands of DBF, EY, EE, TCBF were shifted and the fluorescences of them were quenched. The maximum absorption wavelengths of [Pd(FMTD)]·(HF)2 were located at 541 nm (DBF system),547 nm (EY system),549 nm (EE system),558 nm (TCBF system) and the maximum fluorescence emission wavelengths of them were located at 513～540 nm, the order of quenching values (△F) was DBF>EY>EE>TCBF. The△F was proportional to the FMTD concentration in a certain range and the detection limit was 13.6～29.6 ng/mL. Based on it, a high sensitive, good selective, simple, rapid and new fluorescence quenching method had been proposed to determine FMTD. It can be applied to determine metabolites of FMTD in human urine, which provide reference for pharmacokinetics of the FMTD. The composition and structure of [Pd(FMTD)]·(HF)2 and fluorescence quenching mechanism were fully discussed.4. Determination of chlorpromazine hydrochloride and promethazine hydrochloride by resonance Rayleigh scattering method coupled with flow injection techniqueIn pH 1.0 HCl medium,12-tungstophosphoric acid (TP) reacted with chlorpromazine hydrochloride (CPZ) or promethazine hydrochloride (PMZ) to form ion-association complexes, respectively, which resulted in significant enhancement of the RRS intensity. The maximum peaks were located at 359 nm (TP-CPZ) and 346 nm (TP-PMZ). In a certain range, the RRS intensity was proportional to the concentration of CPZ or PMZ. Based on it, a flow injection analysis (FIA) coupled to resonance Rayleigh scattering (RRS) method was developed for the determination of CPZ and PMZ. The detection limits were 1.7 ng/mL for CPZ and 3.0 ng/mL for PMZ. The reaction conditions and FIA parameters for the systems were optimized. Take TP-CPZ system with high sensitivity as an example, the effect of coexisting substances was investigated, which showed that the method had good selectivity. The proposed method was used for the determination of CPZ in the pharmaceutical formulation and in pig liver with satisfactory results.5. Study on the resonance nonlinear scattering spectra of the interactions of promethazine hydrochloride and chlorpromazine hydrochloride with 12-tungstophosphoric acid and their analytical applicationsIn pH 1.0 HCl medium, TP reacted with PMZ and CPZ to form ion-association complexes respectively, which led to a great enhancement of the resonance nonlinear scattering such as SOS and FDS. Their maximum SOS and FDS peaks were located at 585 nm (TP-PMZ),584 nm (TP-CPZ) and 388 nm (TP-PMZ),329 nm (TP-CPZ), respectively. These results provided some indication for the determination of PMZ and CPZ by SOS and FDS methods. The linear range of TP-PMZ and TP-CPZ systems were 0.0069～2.5μg/mL,0.102～5.0μg/mL (SOS) and 0.079～6.0μg/mL,0.0133～5.0μg/mL (FDS), respectively. The detection limits (3σ) of PMZ and CPZ were 2.08 ng/mL,3.07 ng/mL (SOS) and 2.22 ng/mL,3.98 ng/mL (FDS), respectively. In this work, the optimum reaction conditions, the influences of coexisting substances and ionic strength and analytical application were investigated. The methods have been successfully applied to determination of PMZ and CPZ in tablets. In addition, the composition of ion-association complexes and the reaction mechanism were also discussed. |
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