University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Website: @unf

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Classification: Pharmaceutical -> injection

Citations 21

"Sensitive Assay For Clavulanic Acid And Sulbactam In Pharmaceuticals And Blood Serum Using A Flow Injection Chemiluminometric Method"
Anal. Chim. Acta 2000 Volume 414, Issue 1-2 Pages 15-23
Fatma A. Aly, Nawal A. Alarfaj and Abdulrahman A. Alwarthan

Abstract: A sensitive, simple and inexpensive chemiluminescence (CL) method using flow injection is described for the determination of two β-lactamase inhibitors sulbactam sodium and clavulanic acid (potassium salt) in their pure form, in pharmaceutical preparations and added to blood serum. The method is based on the enhancing effect of these compounds on the CL generated by the oxidation of luminol with hydrogen peroxide in alkaline medium. The CL intensity is a linear function of sulbactam sodium concentration over the range 0.1-150 µg mL-1 with a detection limit (2 x noise) of 0.05 µg mL-1, and for clavulanic acid over the range 0.01-12 µg mL-1 with a detection limit of 0.01 µg mL-1. The method is applied successfully to the determination of the drugs in their dosage forms without interference from co-formulated drugs. The method is specific for the intact drugs in the presence of their degradation products.
Clavulanic acid Sulbactam Chemiluminescence Indirect Optimization Method comparison

"Determination Of Ofloxacin Using A Chemiluminescence Flow Injection Method"
Anal. Chim. Acta 2000 Volume 416, Issue 2 Pages 227-230
Yi Rao, Yan Tong, Xinrong Zhang, Guoan Luo and Willy R. G. Baeyens

Abstract: A new chemiluminescence (CL) flow injection method was proposed for the determination of ofloxacin in pharmaceuticals in the range 0.04-4 µg mL-1 with a detection limit of 0.016 µg mL-1 and a relative standard derivation (RSD) of 2.2% at 0.4 µg mL-1 (n=10). The method is based on the CL reaction of cerium(IV) with sulfite sensitized by ofloxacin. The established procedure could be applied to the determination of ofloxacin in tablet, capsule and injection in agreement with the results obtained by using reported methods.
Ofloxacin Chemiluminescence Method comparison

"Flow Injection Chemiluminescence Determination Of Quinine Using On-line Electrogenerated Cobalt(III) As Oxidant"
Talanta 2000 Volume 51, Issue 3 Pages 515-521
Baoxin Li, Zhujun Zhang and Manli Wu

Abstract: A novel chemiluminescence (CL) flow system for the determination of quinine is described. It is based on the direct chemiluminescence reaction of quinine and cobalt(III) in sulfuric acid medium. The unstable Co(III) was on-line electrogenerated by constant-current electrolysis. The chemiluminescence intensity was linear with a quinine concentration in the range of 0.1-100 µg mL-1. The determination limit was 3.3 x 10^-8 g mL-1. The whole process could be completed in 1 min. The proposed method is suitable for automatic and continuous analysis, and has been applied successfully to the analysis of quinine in pharmaceutical preparation.
Quinine Chemiluminescence Electrochemical reagent generation Method comparison Standard method

"Spectrophotometric Determination Of Cardiac Glycosides By Flow Injection Analysis"
Anal. Chim. Acta 1992 Volume 269, Issue 2 Pages 199-203
P. Solich*, V. Sedliaková and R. Karlíek

Abstract: An optimized flow injection analysis method was described for the determination of lanatoside A, B and C, digoxin, digitoxin, acetyldigitoxin and ouabain, based on their reaction with picric acid in alkaline media and spectrophotometric detection at 486 nm. The flow injection manifold (diagram given) consisted of a FIA 20 Analyser linked to a Zeiss Spekol 10 photometer; the flow rate was 0.6 mL min-1 through the PTFE reaction coil (200 cm) with a sample volume of 100 µL. The calibration graph was rectilinear for 0.025 to 0.5 g L-1 for the cited glycosides (except ouabain) and from 0.01 to 0.2 g L-1 for ouabain; coefficient of variation (n = 6) were 0.6 to 2.2%. Sample throughput was 60 h-1. An optimized flow injection method for the determination of various cardiac glycosides (lanatoside A, B and C, digoxin, digitoxin, acetyldigitoxin, and ouabain) was based on their reaction with picric acid in alkaline media with spectrophotometric detection at 486 nm. The calibration graph was linear for 0.025-0.5 g L-1 cardiac glycosides (except ouabain) and 0.01-0.2 g L-1 ouabain, with relative standard deviation between 0.62 and 2.16% and a sample throughput of 60 h-1. This method was utilized for the determination of digoxin in tablets and lanatoside C, and ouabain in injections.
Glycosides Lanatoside A Lanatoside B Lanatoside C Digitoxin Acetyldigitoxin Digoxin Ouabain Spectrophotometry Optimization

"Flow Injection Chemiluminescence Determination Of Catecholamines With Electrogenerated Hypochlorite"
Anal. Chim. Acta 1998 Volume 374, Issue 1 Pages 105-110
Chengxiao Zhang, Jiachu Huang, Zhujun Zhang,* and Masuo Aizawab

Abstract: A flow injection method for the determination of catecholamines based on the inhibition of the intensity of chemiluminescence from the luminol-hypochlorite system is described. The hypochlorite was electrogenerated online by constant current electrolysis, resulting in the elimination of the instability of hypochlorite solution prepared from commercial available sodium hypochlorite. The detection limits are 6 x 10^-10 g mL-1 for dopamine, 8 x 10^-10 g mL-1 for adrenaline and 8 x 10^-10 g mL-1 for isoprenaline. Linear ranges are 1 x 10^-9 - 2 x 10^-8 g mL-1 for dopamine, 2 x 10^-9 - 2 x 10^-8 g mL-1 for adrenaline, 2 x 10^-9 - 2 x 10^-8 g mL-1 for isoprenaline. The relative standard deviations are <2.8%. The proposed method was applied to the determination of catecholamines in pharmaceutical injections with satisfactory results.
Catecholamines Dopamine Adrenaline Isoprenaline Chemiluminescence Electrochemical reagent generation Indirect

"Immobilization Of Reagents By Polymeric Materials. Determination Of Metamizol"
Talanta 1993 Volume 40, Issue 7 Pages 1067-1071
L. Lahuerta Zamora and J. Martinez Calatayud,

Abstract: Lead dioxide (26.4 g) was stirred with 15.1 g of polyester resin solution (Reposa Al-100) containing low mol. wt. polyester chains and a Co activating agent. Then 0.4 mL of methylethyl ketone was added and stirring was continued until polymerization was complete. The resulting solid was dried in air for 2-3 h, broken into small pieces and ground to a powder in a mechanical grinder. Particles in the size range 200-300 µm were packed in a packed bed reactor (31 cm x 1.5 mm). Metamizole (dipyrone) injections, capsules or solution was dissolved in water and 384.5 µL injected into a 0.1 M HClO4 carrier stream (3 ml/min) for the indirect determination of dipyrone based on the oxidation of dipyrone in HClO4. The resulting Pb(II) was determined by AAS at 217 nm. The calibration graph was rectilinear for 1-6 µg/ml of dipyrone and at 3 µg/ml the RSD was 1.6% (n = 42). Paracetamol interfered seriously but there was no interference from 100 µg/ml of caffeine, dexamethasone or thiamine, 50 µg/ml of lignocaine hydrochloride or pyridoxine, or from 5 µg/ml of ascorbic acid. A method for immobilization of inorganic reagents, based on the dispersion of the reagent into an unsaturated polyester solution is applied to immobilization of lead dioxide. The obtained solid is of application in a flow injection manifold for indirect atomic absorption determination of metamizol in pharmaceutical formulations. The procedure gives a linear calibration graph up to 6 ppm of metamizol with a relative standard deviation of 1.6% (3.0 mg/l) and a sample throughput of 72 hr-1. [References: 9]
Metamizol Spectrophotometry Immobilized reagent Indirect Interferences

"Determination Of Penicillin In Pharmaceutical Formulations By Flow Injection Analysis Using An Optimised Immobilised Penicillinase Reactor And Iodometric Detection"
J. Pharm. Biomed. Anal. 1990 Volume 8, Issue 1 Pages 49-60
M. A. J. van Opstal, R. Wolters, J. S. Blauw, P. C. van Krimpen, W. P. van Bennekom and A. Bult

Abstract: An automated assay for the determination of penicillin in formulations suitable for use in pharmaceutical quality control is presented. The method is based on the classical iodometric penicillin assay which is incorporated in a flow injection analysis (FIA) system. The required hydrolysis is performed online by using an immobilized penicillinase reactor. Packed-bed and single-bead-string enzyme reactors are compared. It turns out that a packed-bed penicillinase reactor (10 cm x 1.5 mm i.d.) provides complete hydrolysis within short residence time, while only little back-pressure is generated. This enzyme reactor is stable for at least 9 months. Enzymatic hydrolysis of the β-lactam ring results in the formation of the corresponding penicilloic acid, which consumes iodine. The iodine consumption is determined colorimetrically by measuring the decrease of the absorbance of the blue colored iodine/starch complex. The optimum reactor length and flow rate for the colorimetrical detection reaction are determined. The optimized method is applied to the assay of penicillin in formulations and the results are compared with the 'true' results obtained with a reference method: a mercurimetric titration. The reliability of the flow injection method is evaluated quantitatively by determining the maximum total error (MTE). The reliability is shown to be highest when measuring at a 0.3-mM level. Eight formulations including capsules, tablets and injectables containing penicillin G, amoxicillin or flucloxacillin are assayed. The MTE does not exceed the 6% level and the most probable MTE is between 1.5 and 3.5%. A 30 µL portion of aqueous penicillin (I) solution was injected into a carrier stream (0.3 mL min-1) of 0.2 M potassium phosphate buffer (pH 6.5) and pumped into a packed-bed immobilized β-lactamase reactor (10 cm x 1.5 mm). The penicilloic acid formed was passed into a single-bead-string reactor (25 cm x 1.5 mm) and mixed with a reagent stream (0.7 mL min-1) of aqueous 0.15% starch solution - (0.5 mM I in 0.5 mM KI) - phosphate buffer (1:1:3). The decrease in absorbance of the blue iodine - starch complex was measured at 590 nm. The calibration graph was rectilinear from 0.1 to 0.5 mM I; the detection limit was 0.025 mM. Results compared well with those obtained by mercurimetric titration. Results are presented for the determination of I in eight formulations, including capsules, tablets and injectables.
Penicillin Spectrophotometry Optimization Immobilized enzyme Automation Enzyme Titrations Buffer pH Calibration Indirect Method comparison

"Investigation Of A New Amoxycillin Sodium Impurity Unstable In Solution"
J. Pharm. Biomed. Anal. 1997 Volume 15, Issue 4 Pages 487-493
L. Valvoa, S. Alimontia, R. Alimentia, C. De Senaa, E. Ciranni Signorettia,*, R. Draiscib and L. Giannettib

Abstract: Injections containing amoxycillin sodium (amoxycillin sodium; I) were dissolved in 0.01 M KH2PO4 of pH 6 (solvent A) to 1 mg/ml or in the solvent contained in the vial (aqueous glycine/sodium hydrate of pH 9.5). Portions were analyzed immediately or at various intervals by HPLC on a 10 µm LiChrosorb RP-18 column (25 cm x 4 mm i.d.) with gradient elution (1 ml/min) using solvent A and acetonitrile/solvent A (4:1; solvent B; 5-70% solvent B in A in 30 min) and detection at 215 nm. The impurities amoxicilloic acid, amoxicillin piperazine-2,5-dione and amoxicillin dimer and tetramer were separated. A novel impurity was also observed when analyzes were carried out within 10 min of dissolution in the vial solvent. Ionspray MS, FIA and HPLC-MS were used to study this impurity which was unstable in aqueous solution (details given). Possible structures are suggested.
Amoxycilloic acid Amoxicillin piperazine-2-5-dione Amoxycillin dimer Mass spectrometry

"Colorimetric Flow Injection Determination Of Resorcinol-type β2-adrenergic Drugs With Phenanthro[9,10-d]imidazole-2-chloroimide"
Anal. Sci. 1989 Volume 5, Issue 5 Pages 513-516

Abstract: For the determination of fenoterol hydrobromide, orciprenaline sulfate or terbutaline sulfate, a portion of ground tablets was extracted with 10 mM HCl (30 ml) by shaking for 10 min. The mixture was diluted with 10 mM HCl to 50 ml, filtered, and the filtrate was diluted 10-fold with water before introduction into the flow injection system; 50 mM borate buffer (pH 11.5) was used as carrier solution (0.8 mL min-1), and reaction with ethanolic 0.003% phenanthro[9,10-d]imidazole-2-N-chloroimide was effected in a 1-m PTFE reaction coil (0.33 mm) at 60°C. Absorbance was measured at 530 nm. Calibration graphs were rectilinear from 0.5 to 200 µM for each drug. Recoveries were >99%; the coefficient of variation (n = 10) were better than 2%. The method was also applied to injection solution and syrup.
Drugs Fenoterol hydrobromide Orciprenaline sulfate Terbutaline sulfate Sample preparation Spectrophotometry Heated reaction Optimization

"Micelle Enhanced Spectrofluorometric Determination Of L-ascorbic-acid Based On Laccase-linked Coupling Reaction Using Flow Injection Stopped-flow Technique"
Anal. Sci. 1997 Volume 13, Issue suppl Pages 67-70

Abstract: A novel spectrofluorimetric method for determination of L-ascorbic acid is described. It is based on the inhibition of L-ascorbic acid on the formation df 2,3-diaminophenazine, which is an oxidation product of o-phenylenediamine catalyzed by laccase, in the presence of Brij-35, which shows strong enhancement on the fluorescence(at lambda em/lambda ex=530 nm/430 nm) of the product, while no effect on the laccase-catalyzed reaction. The mechanism of o-phenylenediamine oxidation reaction catalyzed by laccase in the presence of L-ascorbic acid is discussed. L-ascorbic acid is determined in the range of 0.02 similar to 2.0 µg/ml with a detection limit of 0.014 µg/ml. The method is applied to the determination of L-ascorbic acid in pharmaceuticals, the results agree well with the nominal values and those obtained by the reference method. 20 References
l-Ascorbic acid Fluorescence Catalysis Detection limit Enzyme Method comparison Redox Standard method Micelle Stopped-flow

"An Aluminum Fluorescence Sensing Layer Based On 2-(diethylamino)ethyl Sephadex As A Substrate"
Fenxi Huaxue 1996 Volume 24, Issue 10 Pages 1129-1132
Lu, J.Z.;Zhang, Z.J.;Shen, A.B.

Abstract: Salicylfluorone (I) was immobilized on DEAE Sephadex (II) by stirring a mixture of 10 mL ethanolic 0.3 mM I and 0.1 g II for 20 min. The res2O. It was then injected into a flow cell for determination of Al in water and glucose injection samples by fluorimetry at 542 nm (excitation at 350 nm). A HCl/acetate buffer of pH 6 was used for the determination (0.5 ml/min) and EDTA solution was used to regenerate the sensor. The calibration graph was linear from 20-150 ng/ml of Al. Recoveries were 97-105% and RSD (n = 7) were Total analysis time was 1 min. Tolerance levels are given for twenty four foreign ions (listed), Cu(II) and Fe(III) did not cause any interference.
Aluminum Fluorescence Interferences Sephadex Immobilized reagent

"Flow Injection Photochemical Spectrophotometric Determination Of Chlorpromazine In Pharmaceutical Preparations"
Fenxi Huaxue 1997 Volume 25, Issue 5 Pages 573-575
Zhu, J.P.;Chen, H.W.;Fang, Q.J.

Abstract: Sample from chlorpromazine hydrochloride (I) injection solution was diluted with water to a concentration of 12.5 mg/l. A 2 mL portion of the diluted solution was treated with 1 mL 0.1 M HCl and the solution was diluted to 25 mL with water. Portions (250 µL) were injected a carrier stream of water at 2.1 ml/min in a flow injection manifold (diagram illustrated). The stream was carried to a knotted reactor (coiled around a fluorescent lamp) for photochemical reaction by UV irradiation from the lamp at 365 nm. The fluorescence intensity of the reaction product was measured online at 374 nm (excitation at 253 nm). The calibration graph was linear from 10^-600 µg/l of I with a detection limit of 5.4 µg/l. The RSD was 0.5%. No interference was observed from 0.5-fold ascorbic acid and Na2SO3, 100-fold sorbitol and 250-fold glucose. Sampling frequency was 90 runs per h. The method was also applied to the analysis of I in tablets.
Chlorpromazine Fluorescence Interferences Photochemistry Knotted reactor

"Flow Injection Chemiluminescence Determination Of Methotrexate"
Fenxi Huaxue 1998 Volume 26, Issue 9 Pages 1136-1138
He, Y.;Xue, Y.;Feng, M.L.;Lu, J.

Abstract: The chemiluminescence reaction of methotrexate (MTX)-potassium permanganate with formaldehyde as an enhancer was investigated by the flow injection system. A new method for the determination of MTX on the basis of the reaction was reported. The detection limit is 3.4 x 10^-9 g/mL, the relative standard deviation is 1.1% (2.0 x 10^-6 g/mL MTX, n = 11). The linear range is 1.0 x 10^-8 ~ 1.0 x 10^-5 g/mL. The method has been applied to the determination of MTX in the MTX injection and tablet.
Methotrexate Chemiluminescence

"Determination Of Vitamin B6 By Flow Injection Chemiluminescence Method"
Fenxi Shiyanshi 1998 Volume 17, Issue 3 Pages 5-8
Li, L.;Yang, M.;Feng, M.L.;Lu, J.

Abstract: A new flow injection chemiluminescence method for the determination of vitamin B6 with the system of KMnO4-Na2S2O4-VB6 was established. Strong chemiluminescence signal was observed when the mixed solution of Na2S2O4 and sample was injected into the acidic KMnO4 solution in a flow-cell. The linear range for the determination of VB6 is 1 x 10^-4 ~ 8 x 10^-2 g/L. The detection limit is 5.8 x 10^-8 g/L, the relative standard deviation is 1.1% for 11 measurements of 4.0 x 10^-3 g/L standard solution The recommended method has been successfully used for the determination of VB6 in tablet and injection.
Vitamin B6 Chemiluminescence

"Determination Of Alkylating Antitumor Drugs By Flow Injection Analysis"
Iyakuhin Kenkyu 1987 Volume 15, Issue 5 Pages 749-752
Suzuki, Masao; Nishinaka, Tomoko; Takitani, Shoji (SFS)

Abstract: The alkylating antitumor drugs carboquone, cyclophosphamide, thiotepa, busulfan, and melphalan in commercial preparations (powders, tablets, or injections) were dissolved in suitable solvents and determined by spectrometry with the flow injection system, using 4-(4-nitrobenzyl)pyridine as reactant and detection at 580 nm. This method is simple and fast, and the results are comparable with those from other methods (HPLC, gas chromatography, etc.). (SFS)
Drugs Carboquone Thiotepa Busulfan Melphalan Cyclophosphamide Busulfan Spectrophotometry Method comparison

"Studies On Fluorimetric Determination Of Cyclophosphamide With Nicotinamide And Acetophenone"
Iyakuhin Kenkyu 1985 Volume 16, Issue 5 Pages 1136-1141
Takitani, Shoji; Suzuki, Masao; Takamatu, Motonobu; Murayama, Mitunori; Sano, Akira (SFS)

Abstract: Fluorometric determination of cyclophosphamide (I) [50-18-0] was performed by a manual method and flow-injection anal. with nicotinamide [98-92-0] and acetophenone [98-86-2]. In manual analysis, a 100 mL sample was treated with 500 mL nicotinamide solution (5%(w/v)) at 100°C for 60 min, and the reaction mixture was cooled, mixed with 500 mL acetophenone solution (2%(v/v)) and 500 mL KOH (0.5N in 50% EtOH), allowed to stand for 15 min and treated with 1.5 mL formic acid solution (60%) at 100°C for 3 min for the measurement of the fluorescence intensity (relative to standard quinine solution) at 440 nm with excitation at 385 nm. In the second analysis, a flow-injection system with FP110-type fluorometric detector was used. The calibration curve was linear in the range of 0.02-30 mg/100 mL for the manual analysis and of 0.98-16,000 ng/mL for the flow-injection analysis. The relative standard deviation was 2.37-5.16 and 1.23-3.30%, respectively. The methods were used in the determination of I in pharmaceutical preparations (injections, tablets). The flow-injection method was rapid (20 samples/h) and highly reproducible. (SFS)
Cyclophosphamide Fluorescence Method comparison

"Determination Of Analgin By Flow Injection Analysis With Chemiluminescence Detection"
Shaanxi Shifan Daxue Xuebao (Ziran Kexue Ban) 1998 Volume 26, Issue 3 Pages 68-70
Li Liqing, Nie Feng, Yang Minli, Feng Manliang, Lu Jiuru

Abstract: A new method for the determination of analgin in tablets and injections by using flow injection chemiluminescence was based on the chemiluminescence reaction of analgin-KMnO4. The main factors which affect the determination were investigated. Under optimum conditions, the linear range for the determination of analgin was 1 x 10^-7-8 x 10^-5g/mL, the determination limit was 4.2 x 10^-8 g/mL.
Analgin Chemiluminescence Optimization

"Chemiluminescence Determination Of Sodium Nitroprusside By Flow Injection Analysis"
Yaowu Fenxi Zazhi 1997 Volume 17, Issue 2 Pages 75-77
Li Jianzhong, Wang Tieling

Abstract: Sample was dissolved in 0.5 mL 2 M NaOH and diluted with water to 25 mL. After 1 min, a 100 µL portion of the solution was injected into the flow injection manifold (diagram shown) into a stream of NaHCO3/Na2CO3 buffer of pH 12 and mixed with reagent streams of 1 mM luminol and 50 mM H2O2 pumped at 3 ml/min and the chemiluminescence intensity was measured. The calibration graph for sodium nitroprusside (I) was linear from 0.2 µM to 0.1 mM with a detection limit of 9 nM. Copper(II), oxalate and ascorbic acid interfered. Sampling frequency was 40 runs per h. The method was applied to the analysis injection solutions containing I, with recovery of 98.5-101% and RSD of 1-1.2%. Results agreed closely with those obtained by the method published in the Chinese Pharmacopoeia.
Nitroprusside Chemiluminescence Method comparison Interferences Standard method

"Flow Injection Analysis Of Mitomycin-C In Flacons"
J. Liq. Chromatogr. Relat. Technol. 2005 Volume 28, Issue 4 Pages 619-629
Arin Gul Dal, Dilek Dogrukol-Ak, Muzaffer Tuncel

Abstract: A precise and accurate flow injection analysis (FIA) method for the determination of mitomycin-C (MMC) in pharmaceutical flacons is described. Britton-Robinson (BR) buffer at pH 7.0 was used as a carrier solvent at a flow-rate of 1.0 mL min-1. MMC signals were detected at 363 nm using a UV-spectrophotometric detector. The intra- and inter-assay precisions were less than 2.0%. The calibration curves were also linear in the concentration range of 2.0 x 10^-6 - 1.0 x 10^-5 M for intra- and inter-day studies with high correlation coefficients. The limit of detection (LOD) and limit of quantification (LOQ) values were found to be 1.93 x 10^-8 and 6.45 x 10^-8 M, respectively. The results obtained with the application of the method were compared with those of high performance liquid chromatography (HPLC) and UV-spectrophotometry. It was found that there was insignificant difference between the methods.
Mitomycin C Spectrophotometry Method comparison

"Chemiluminescence Of Cobalt(II)-catalysed Auto-oxidation Of Sulphite And Its Application To Cobalt Analysis"
Luminescence 2004 Volume 19, Issue 5 Pages 253-258
Xiao-Feng Yang, Hua Li*

Abstract: The oxidation of sulphite by dissolved oxygen in aqueous solution catalyzed by cobalt(II) was investigated. A weak chemiluminescence (CL) emission was observed when the reaction took place in a strong alkaline solution without any special CL reagent. Further studies showed that in the presence of fluorescein sodium the CL signal was enhanced significantly. The CL emission is linear with Co(II) concentration in the range 0.6-80 nmol/L and the detection limit is 0.3 nmol/L. In addition to Co(II), other transition metal ions were also tested, and the results showed that the proposed system was highly selective for Co(II). The method was successfully applied to the determination of Co(II) in pharmaceutical preparations. The possible CL mechanism was also discussed.
Cobalt(II) Chemiluminescence Selectivity Interferences

"Determination Of Kanamycin Using Flow Injection Analysis Coupled With Resonance Rayleigh Scattering Detection"
Bull. Chem. Soc. Jpn. 2006 Volume 79, Issue 2 Pages 247-251
Xiaoli Hu, Shaopu Liu and Zhongfang Liu

Abstract: A flow injection analysis (FIA) method coupled with resonance Rayleigh scattering (RRS) detection for the determination of kanamycin sulfate (KANA) was developed. The method is based on the ion-association reaction of KANA with acid triphenylmethane dyes such as aniline blue W. S (AB) and methyl blue (MB) by virtue of electrostatic and hydrophobic interaction forces, which results in a significant enhancement of RRS intensity; their maximum scattering peaks are all at 346 nm. The optimum conditions of the reactions and the flow-through parameters including the length of reaction tubing, the flow rate of the carrier stream and the sample injection volume are discussed in this paper. Under the optimum experimental conditions, the linear ranges for both systems are 0.02-12.0 µg mL-;1. The detection limits (3s) are 4.2 ng mL-;1 for the AB system and 5.0 ng mL-;1 for the MB system and the relative standard deviation for 9 replicate measurements of 2.0 µg mL-;1 KANA solution was 1.1%. The proposed method was successfully applied to the determination of KANA in commercial KANA injection, urine and serum samples, and the sample throughput was 30 h-;1.
Kanamycin Raman Optimization