Determination of Gossypol in Trace Level by Flow Injection Analysis with Chemiluminescence Detection

This work reports the single-molecule detection of gossypol by flow injection analysis with chemiluminescence method. The method is based on the reaction of luminol with ferricyanid in sodium hydroxide medium sensitized by gossypol. Under the optimum conditions, the CL intensity is proportional to the concentration of gossypol over the range of 1.11×10^-17-2.78×10^-16 mol/L in acid solution and 8.00×10^-11-7.39×10^-8mol/L in neutral solution with correlation coefficients 0.9983 and 0.9905, respectively. The detection limits is 1.60×10^-18 mol/L （S/N=3）. The proposed method has been applied for the determination of the gossypol in cottonseeds and pharmaceutical formulations with satisfactory results.

Determination of chlorogenic acid by flow injection irreversible biamperometry

A flow injection irreversible biamperometric method for the determination of chlorogenic acid is described. The proposed method is based on the electrochemical oxidation of chlorogenic acid at pretreated platinum electrode and the reduction of permanganate at another electrode to form an irreversible biamperometric detection system. Under the external potential difference （z^v） of 0 V, in the 0.05 mol/L sulfuric acid, chlorogenic acid can be determined over the range 0.8-120 mg/L with a sample measurement frequency of 80 samples/h. The detection limit is 0.18 mg/L. The proposed method exhibits the satisfactory reproducibility with a relative standard derivation （R.S.D.） of 2.21% for 19 successive determinations of 40 mg/L.

Determination of Ciprofloxacin by Flow Injection Analysis Based on Chemiluminescence System

A novel flow injection chemiluminescence （CL） method for the determination of ciprofloxacin （CPLX） was reported. The proposed method is based on luminescence produced by KMnO4-Na2S2O4-Tb^3＋-CPLX chemiluminescence （CL） system. The effects of some critical experimental conditions were discussed and the optimization of working conditions was investigated. The linear dynamic range is 3.00 × 10^-8 - 9.00 × 10^-7 mol ·L-1 and the detection limit for CPLX is 4.40 × 10^-9 mol·L^-1. This method was applied to the determination of CPLX in tablet, urine, and serum samples and the recoveries of real sample analyses were in the range from 110 ± 4 to 104 ± 4.

Study on Chemiluminescence Reactions of L ucigenin and Reductants by Flow Injection Analysis

The chemiluminescence reactions between lucigenin and reductants such as Mo(LII),V( II), U(III), W(III), Cr(II), Ti(III) and Fe( II), which were produced on-line by passing Mo(VI),V(V),U(VI), W(VI), Cr(VI,III),Ti(IV) and Fe(III) through a micro Jones column, are studied in detail. Results show that the reactions can be used directly for the determination of these substances. The mechanism of the reactions is also investigated.

On-line Preconcentration and Determination of Trace Metals in Water Samples by Flow Injection Combined with Flame Atomic Absorption Spectrometry via Calix[4]arene Carboxylic Acid Packed Micro-column

An adsorbent calix[4]arene carboxylic acid was employed as the adsorption material for on-line flow in jection（FI） micro-column preconcentration coupled with flame atomic absorption spectrometry（FAAS） determination of trace heavy metals（Cu, Pb, Co, Ni and Cd）. Parameters such as the pH, loading time and flow rate of sample, and the concentration, volume and flow rate of eluent were optimized. The enrichment factors are 50.0, 56.5, 11.6, 12.1 and 19.1 for Cu, Pb, Co, Ni, and Cd, respectively, and a sample throughput of 20 h–1 was obtained. The limits of de tection for Cu, Pb, Co, Ni, and Cd were in a range of 1.56―3.91 μg/L, and the relative standard deviations（RSDs） were less than 2.76%（n=7）. Furthermore, the proposed method was successfully applied to the determination of Cu, Pb, Co, Ni, and Cd in certified reference materials and various water samples.

Flow Injection Chemiluminescence Analysis of Low Level Concentration of Hydrazine

Combined with flow-injection (FI) technology, a simple chemiluminescence (CL) method was developed for hydrazine determination in this paper. It was found that hydrazine could greatly decrease the strong CL signal produced by the reaction between luminol and hexacyanoferrate (III) in alkaline medium. The decreased CL intensity was linear with hydrazine concentration in the range of 5.0×10-9 g·mL-1 to 4.0×10-5 g·mL-1, and the limit of detection was 2.0×10-9 g·mL-1 (3σ) with a relative standard deviation of 2.4~4.1% (n=5).

Flow injection spectrophotometric determination of vitamin E in pharmaceuticals,milk powder and blood serum using potassium ferricyanide-Fe(Ⅲ) detection system

A simple and sensitive flow injection spectrophotometric method is reported for the determination of vitamin E using potassium ferricyanide-Fe(Ⅲ) detection system.In the presence of vitamin E,Fe(Ⅲ)/ferricyanide reduces.The in situ reduced ions are then reacted with unreduced portion of ferricyanide/Fe(Ⅲ) to make soluble Prussian blue,which is monitored at absorption wavelength of 735 nm.Linear calibration graph was obtained in the concentration range of 0.1-40μg mL^(-1).The relative standard deviations (n=4) were in the range of 1.1-3.6%,with limits of detection(3 s blank) of 0.04μg mL^(-1).The proposed method allowed 12 injections h^(-1).The method is applied to determine vitamin E in pharmaceuticals,infant milk and blood serum samples using hexane extraction with the recoveries in the range of 93±3 to 97.5±4%.The method is validated using certified reference materials SRM 968c for blood serum samples.

Numerical Study on the Effects of Contraction Ratio in a Two-Phase Flow Injection Nozzle

The Euler-Euler numerical method was used to investigate the effects of contraction ratio on twophase flow mixing with mass transfer in the flow injection nozzle. The geometric shape of the nozzle was modified to improve carbonation efficiency. A gas inlet hole was created to increase the flow mixing of CO2 with water. A nozzle throat was also introduced to increase the gas dissolution by increasing flow rates. Various contraction ratios of nozzle throat, inlet gas and liquid velocities, and gas bubble sizes were employed to determine their effects on gas hold-up, gas concentration, and mass transfer coefficient. Results revealed that the flow injection nozzle with high contraction ratios improved carbonation because of high gas hold-up. Gas concentration was directly related to contraction ratio and gas flow velocities. Carbonation reduced when high liquid velocities and large gas bubbles were employed because of inefficient flow mixing. This study indicated that flow injection nozzle with large contraction ratios were suitable for carbonation because of their ability to increase gas hold-up, gas concentration, and mass transfer coefficient.

Kinetic-spectrophotometric determination of free cyanide by stopped-flow reversed flow injection analysis

A stopped-flow reversed flow injection method for the determination of free cyanide is proposed. Pyridine-barbituric acid mixture is injected in the flow system as reagent to form the colour species with cyanide. The flow is stopped when the reagent zone comes in the flow cell, where absorbance-time data are collected at 580nm wavelength. The linear range of the determination is 0.1 -10μg/ml CN-. The sampling rate is 60h-1 and the relative standard deviation is 1.6% (n=16) at 5.0 μg/ml CN-1 level. With satisfactory results, the proposed method was applied to the determination of free cyanide in wastewater without sample pretreatment.

Study on Quenching Effect of Holmium (Ⅲ) Ion in Chemiluminescence System of Luminol H_2O_2-Cr(Ⅲ) by Flow Injection Technique

A new chemiluminescence (CL) analytical method for determination of rare earth Ho(Ⅲ) ion is reported. It is based on the quenching effect of Ho(Ⅲ) ion on CL intensity of Luminol H 2O 2 Cr(Ⅲ) system. The detection limit is 3×10 -8 mol/L, the linear range is from 1×10 -7 to 1×10 -4 mol/L; the relative standard deviation is less than 3% (for 2×10 -7 mol/L Ho, n=11). The method was applied to determination of Ho(Ⅲ) in pure samples with satisfactory results.

O-(β-hydroxyethyl)rutosides determination by micellar flow injection(FI)-spectrofluorimetry

A simple,eco-friendly.sensitive and economic flow injection spectrofluorimetric method was developed for the determination of O-（β-hydroxyethyl）rutosidcs.The procedure was based on the use of an anionic surfactant such as sodium dodecyl sulfate to provide an appreciable O-（β-hydroxyethyl）rutosides fluorescence enhancement,increasing considerably the sensitivity of detection.All the variables affecting the fluorescence intensity were studied and optimized.The flow rate was 5 mL/min with detection at 450 nm（after excitation at 346 nm）.A linear correlation between drug amount and peak area was established for 0-（β-hydroxyethyl）rulosides in the range of 0.01-200 μg/mL with a detection limit of0.001 μg/mL（s/n = 3）.Validation processes were performed by recovering studies with satisfactory results.The new methodology can be employed for the routine analysis of 0-（P-hydroxyethyl）rutosides in bulks as well as in commercial formulations.

Flow Injection Analysis of Histidine with Enhanced Electrogenerated Chemiluminescence of Luminol

A simple and sensitive flow injection method is presented for the determination of histidine based on its enhancement of electrogenerated chemiluminescence (ECL) of luminol. After optimization of the experimental parameters, the working range for histidine was in 1.0 x 10-6 to 1.0 x 10 -3 mol/L with a detection limit (S/N = 3) of 0.56 mmol/L. The relative standard deviation was 1.6% for 11 measurements of 5 x 10 5 mol/L histidine solution. The proposed method has been successfully applied to the determination of histidine in real pharmaceutical preparation.

Studies on Combination of Flow Injection and Microwave Plasma Torch-Atomic Emission Spectrometry

Although the flow injection(FI) as a sample introduction technique has been extensively applied to atomic spectrometry, such as ICP-AES and AAS, very little has been done so far on coupling FI to microwave plasma systems. Gehlausen et al. determined aqueous fluorine by coupling flow injection analysis (FIA) with HeMIP

Study on the Flow Injection Micro-Column Pre-Separation System Coupled With High Performance Liquid Chromatography for the Determination of Ecdysterone in Traditional Chinese Medicine

A flow injection (FI) micro-column system coupled with high performance liquid chromatography (HPLC) was proposed for the pre-separation and determination of active organic component (ecdysterone) in traditional Chinese medicine, Loulu. The factors influencing separation performance were investigated and optimized. Under the optimal conditions, the contents of ecdysterone in Loulu were determined by HPLC system using MeOH-H_2O (40: 60,V/V) as the mobile phase at a flow rate of 1. 0 mL/min. The calibration curve was linear in the range of 0. 5~ 100 mg/L of ecdysterone concentrations. The detection limit of the analyte was 0. 11mol/L(3) with a precision of 0. 38% RSD (n=7 f c= 10. 0 mg/L). The average recovery of the method was 98. 7%. The proposed method has been applied to determine ecdysterone in practical samples, and the determined values by both external standard method and standard addition method were in good agreement. Compared to the traditional solid extraction method, the system proposed has the advantages of simple procedure, good reproducibility, minimum volume requirement, reduction of matrix interference and low contamination risk.

SELECTIVE SULFUR DIOXIDE DETERMINATION BY GAS DIFFUSION FLOW INJECTION ANALYSIS WITH CHEMILUMINESCENT DETECTION

Sulfur dioxide has been found to decrease the chemiluminescence of luminol-iodine system.A new determination method for sulfur dioxide in atmosphere is developed by applying this reaction to a flow injection gas diffusion separation system.This permits the determination of sulfur dioxide selectively and rapidly.

Normal and reverse flow injection-spectrophotometric determination of thiamine hydrochloride in pharmaceutical preparations using diazotized metoclopramide

Simple and sensitive normal and reverse flow injection methods for spectrophotometric determination of thiamine hydrochloride （THC） at the microgram level were proposed and optimized. Both methods are based on the reaction between THC and diazotized metoclopramide in alkaline medium. Beer＇s law was obeyed over the range of 10 300 and 2-90 ug/mL, the limits of detection were 2.118 and 0.839 ug/mL and the sampling rates were 80 and 95 injections per hour for normal and reverse flow injection methods respectively. The application of both methods to commercially available pharmaceuticals produced acceptable results. The flow system is suitable for application in quality control processes.

Determination of ribavirin by flow injection chemiluminescence

Objective： To establish a rapid and precise continuous flow-injection chemiluminescence （CL） method to determine ribavirin. Methods： The ribavirin could restrain strongly CL reaction of luminol in sodium hydroxide （NaOH） solution with potassium chlorate （KClO3）. The different experimental parameters affecting the CL intensity were studied carefully. Results： Under optimum conditions （The concentrations of luminol, KClO3, and NaOH were at 0.1 mmol/L, 0.5μmol/L, and 0.2 mol/L, respectively）, the linear range of the working curves was 0.01-7.00μg/ml with a detection limit of 0.004μg/ml. Conclusion： The method is simple, rapid and sensitive, and successfully applied to the determination of ribavirin in pharmaceutical preparations and biological fluids.

Flow Injection Chemiluminescence Determination of 4-methylsalicylic

As potassium bichromate can be reduced by 4-methysalicylic acid to chromium(III) which enhance the CL intensity of luminol-H2O2 system,a new chemiluminescence system for the determination of 4-methysalicylic acid has been established.The relative CL intensity was correlated with salicylic acid concentration in the range 7.0×10-9～8.0×10-6 mol/L,and the detection limit was 1.0×10-9 mol/L.The relative standard deviation(n=8) for 4.0×10-7 mol/L 4-methysalicylic acid is 2.9%.The method has been applied to the determination of 4-methysalicylic acid in the bactericidal solutions with satisfactory results.

Linde Type a Zeolite and Type Y Faujasite as a Solid-Phase for Lead, Cadmium, Nickel and Cobalt Preconcentration and Determination Using a Flow Injection System Coupled to Flame Atomic Absorption Spectrometry

In this work, a flow injection analysis (FIA) method for the trace determination of lead, cadmium, nickel and cobalt in natural waters by formation of neutral chelates with ammonium pyrrolidine dithiocarbamate (APDC) was developed. The neutral chelates formed was retained in a mini-column packed with Linde type A zeolite (LTA) and type Y Faujasite zeolite (FAU) and then eluted with methyl isobutyl ketone (MIBK) to flame atomic absorption spectrometry (EAA) for its detection. Physicochemical characterization of this zeolite was carried out by Fourier Transform infrared spectroscopy and attenuated total reflectance (FTIR and IR-ATR), scanning electron microscopy and energy dispersive X-ray microanalysis (SEM-EDX) and X-ray power diffraction (XRD). Then, a FIA configuration was used with a column preconcentration system coupled to the detection system at room temperature (22?C). The detection limit and the relative standard deviation for 5 determinations of different solutions of Pb2+, Co2+, Ni2+ and Cd2+ for FAU and LTA zeolite were calculated. The sampling frequency ranged from 18-35 h-1 and preconcentration factors from 21-250 were achieved, for a sample volume of 6 mL using 20 mg of sorbents, indicating a high retention of the analytes on the zeolites material. The recoveries obtained in natural waters samples were close to 100% for all ions metal using synthetic zeolites, confirming the applicability of the method. The isotherm models of Langmuir, Scatchard, Freundlich and Dubinin-Radushkevich were used to study the equilibrium data, indicating that successfully followed the Freundlich and Dubinin-Radushkevich (D-R) isotherms at low metal ion concentration. The Freundlich parameter n varied between 0.35-1.01, whereas D-R isotherm yields the sorption free energy E 8 kJ.mol-1 indicating psysisorption.