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.

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.

Reversed flow injection spectrophotometric determination of low residuals of chlorine dioxide in water using chlorophenol red

A novel, simple, rapid, sensitive and highly selective flow injection procedure for the spectrophotometric determination of chlorine dioxide in the presence of other chlorine species, viz,free chlorine, chlorite, chlorate and hypochlorite, is developed. The method is based on the discoloration reaction between chlorine dioxide and chlorophenol red and can overcome the shortcomings existed in direct spectrophotometric determination for chlorine dioxide owing to the serious interference of free and combined chlorine. The procedure gave a linear calibration graph over the range 0—0.71 mg/L of chlorine dioxide. With a detection limit of 0.024 mg/L and a sample throughput of 60 samples/h.

Flow-injection Determination of Cysteine,N-Acetyl Cysteine and Glutathione in Pharmaceuticals via Potassium Ferricyanide-Fe(Ⅲ) Spectrophotometric System

A simple flow injection spectrophotometric method is reported for the determination of cysteine,N-acetyl cysteine and glutathione based on the reduction of Fe（Ⅲ）/ferricyanide,the in situ reduced ions are reacted with unreduced portion of ferricyanide/Fe（Ⅲ） to form soluble Prussian blue,which is monitored at 735 nm.The calibration graphs are linear in the concentration ranges of（1―100）×10-6 mol/L for cysteine and N-acetyl cysteine,and（1―50）×10-6 mol/L for glutathione.The relative standard deviations of 1.8%,2.5% and 1.9% were found for eleven replicate analyses of 5×10-6 mol/L cysteine,N-acetyl cysteine and glutathione.The limits of detection（3σ blank） at 5×10-7 mol/L for cysteine,and 3×10-7 mol/L for N-acetyl cysteine and glutathione were obtained.The proposed method allowed 60 injections/h.The effects of common substances present in pharmaceuticals and human physiological fluids were examined.The method was applied to determining cysteine in pharmaceutical formulations with the recoveries in a range of 97% to 106% and the results obtained are agreed well with labeled values.

Flow-injection Spectrophotometric Determination of Uric Acid in Urine via Prussian Blue Reaction

A simple and sensitive flow injection（FI） spectrophotometric method was reported for the determination of uric acid based on the reduction of Fe（III）/ferricyanide in the presence of uric acid. The in situ reduced ions reacted with unreduced portion of ferricyanide/Fe（III） to form soluble Prussian blue, which was monitored at an absorption wavelength of 735 nm. The optimized conditions allow a linear calibration graph in a concentration range of 1―100 μmol/L. The relative standard deviation was in a range of 0.5%―2.5%, with a detection limit（3σ blank） of 0.3 μmol/L and a sampling frequency of 60 injection/h was obtained. The effect of common substances present in human physiological fluids on the determination of uric acid was examined. The method was applied to determining uric acid in human urine samples with the recoveries in a range of 96%―105%. The results agree well with those by spectrophotometric reference method at a confidence level of 95%. Spectrophotometric procedures for uric acid determination in clinical samples were reviewed briefly.

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).

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.

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.

The Determination of Iodide Based on a Flow-injection Coupling Irreversible Biamperometry

A novel flow-injection irreversible biamperometric method is described for the direct determination of iodide. The method is based on electrochemical oxidation of iodide at the gold electrode and the reduction of permanganate at the platinum electrode to form an irreversible biamperometric detection system. Under the applied potential difference of 0 V, in the 0.05 mol/L sulfuric acid, iodidecan be determined over the range 4.00×10^-7-1.00×10^-5 mol/L with a sampling frequency of 120 samples per hour. The detection limit for I- is 3.0×10^-7 mol/L and the RSD for 40 replicate determinations of 4.0×10^-5 mol/L potassium iodide is 1.68%. The new method was applied to the analysis of iodide in table salt with satisfactory results.

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.

Determination of Trace Non Rare Earth Elements in High Purity Rare Earth Oxides by ICP－AES with Microcolumn Preconcentration in a Flow Injection System

A new method for the determination of trace non-rare earth elements in high purity rare earth oxides by ICP-AES with preconcentration on an active carbon-silica gel microcolumn in a flow injection system is described in this paper. Experimental parameters such as pH, flow rate,reagent concentration,length of reaction coil,eluent acidity,etc. were optimized. In the buffer solution of NH3. H2O/NH4Cl at pH 4. 6,Al,Cr,Cu,Fe, Pb, V and Zn can be preconcentrated and then eluted with 4. 5 mol/L nitric acid utilizing stop-flow technique. The enrichment factors were in range of 8. 1￣12. 6 with detection limits of μg/m level ,and the RSD with metals at μg/g level were 2. 3￣5. 0% (n= 7). The method proposed can reduce the matrix interference effectively , and has been applied to the determination of non-rare earth metals atμg/g level in high purity Eu2O3 with satisfactory results.

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.

Flow-injection spectrophotometric determination of vanadium with malachite green oxalate by bromate in acidic and micellar medium

A flow injection method is proposed for determining vanadium（V）. The method is based on its catalytic effect on the oxidation of malachite green oxalate by bromate. The reaction was monitored spectrophotometrically by measuring malachite green oxalate absorbance at λmax = 625 nm. The reagents and manifold variables, which have influences on the sensitivity, were investigated and the optimum conditions were established. The optimized conditions made it possible to determine vanadium in the ranges of 10-140 ng/mL with a detection limit of 5.2 ng/mL and a sample rate of 20 ± 5 samples/h.

Determination of Lanthanu m in Lu minol- H_2 O_2- Cr( Ⅲ) Syste m by Flow Injection Chemilu minescence

A novel method of flow injection chemiluminescence (CL) analysis for the determination of rare earth La(Ⅲ) ion is prensented. It is based on the quenching effect of La(Ⅲ) ion in the CL system of Luminol H 2O 2 Cr(Ⅲ). The CL emission intensity is linear with La(Ⅲ) concentration in the range 1×10 -7 ～1×10 -4 mol/L; the detection limit is 4×10 -8 mol/L, the relative standard deviation is less than 3% (for 2×10 -7 mol/L La, n =11).

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.

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.