Flow injection chemiluminescence determination of naproxen based on KMnO4-Na2SO3 reaction in neutral aqueous medium

A simple, rapid and sensitive flow injection chemiluminescence (CL) method is described for the determination of naproxen. It was found that strong CL signal was generated when naproxen was mixed with KMnO₄ and Na₂SO₃ in neutral aqueous medium. Under the optimum experimental conditions, the CL intensity was linearly related to the concentration of naproxen from 4.0 × 10⁻⁹ to 1.0 × 10⁻⁶ g mL⁻¹ (r = 0.9993). The detection limit was 2 × 10⁻⁹ g mL⁻¹ naproxen, the relative standard deviation for 1.0 × 10⁻⁷ g mL⁻¹ naproxen solution was 1.5% (n = 11) and the sampling frequency was 120 h⁻¹. The method was applied to the determination of naproxen in pharmaceutical preparation with satisfactory results. The mechanism of CL reaction was discussed briefly.     

Determination of indole-3-acetic acid and indole-3-butyric acid in mung bean sprouts using high performance liquid chromatography with immobilized Ru(bpy)3-KMnO4 chemiluminescence detection

A novel method for determination of indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA) in an extract from mung bean sprouts using high performance liquid chromatography (HPLC) with chemiluminescence (CL) detection is described. The method is based on the CL reaction of auxin (indole-3-acetic acid and indole-3-butyric acid) with acidic potassium permanganate (KMnO₄) and tris(2,2′-bipyridyl)ruthenium(II), which was immobilized on the cationic ion-exchange resin. The chromatographic separation was performed on a Nucleosil RP-C18 column (i.d.: 250 mm × 4.6 mm, particle size: 5 μm, pore size: 100) with an isocratic mobile phase consisting of methanol-water-acetic acid (45:55:1, v/v/v). At a flow rate of 1.0 mL min⁻¹, the total run time was 20 min. Under the optimal conditions, the linear ranges were 5.0 × 10⁻⁸ to 5.0 × 10⁻⁶ g mL⁻¹ and 5.0 × 10⁻⁷ to 1.0 × 10⁻⁵ g mL⁻¹ for IAA and IBA, respectively. The detection limits were 2.0 × 10⁻⁸ g mL⁻¹ and 2.0 × 10⁻⁷ g mL⁻¹ for IAA and IBA, respectively. The relative standard deviation (RSD) of intra-day were 3.1% and 2.3% (n = 11) for 2 × 10⁻⁶ g mL⁻¹ IAA and 2 × 10⁻⁶ g mL⁻¹ IBA; The relative standard deviations of inter-day precision were 6.9% and 4.9% for 2 × 10⁻⁶ g mL⁻¹ IAA and 2 × 10⁻⁶ g mL⁻¹ IBA. The proposed method had been successfully applied to the determination of auxin in mung bean sprouts.     

Flow injection chemiluminescence determination of nitrofurazone in pharmaceutical preparations and biological fluids based on oxidation by singlet oxygen generated in N-bromosuccinimide-hydrogen peroxide reaction

A simple flow injection chemiluminescence (FI-CL) method was proposed for the determination of nitrofurazone. Strong CL signal was generated during the reaction of nitrofurazone with H₂O₂ and N-bromosuccinimide (NBS) in alkaline condition. The CL signal was proportional to the nitrofurazone concentration in the range 1.0 × 10⁻⁷ to 1.0 × 10⁻⁵ g mL⁻¹. The detection limit was 2 × 10⁻⁸ g mL⁻¹ nitrofurazone and the relative standard deviation was less than 4% (6.0 × 10⁻⁶ g mL⁻¹ nitrofurazone, n = 11). The proposed method was successfully applied to the determination of nitrofurazone in compound furacillin nasal drops, human plasma and urine samples. The CL reaction mechanism was also discussed briefly. Singlet oxygen generated in the reaction between H₂O₂ and NBS was suggested to be participated in the CL reaction.     

β−cyclodextrins-based inclusion complexes of CoFe2O4 magnetic nanoparticles as catalyst for the luminol chemiluminescence system and their applications in hydrogen peroxide detection

β−cyclodextrins (β−CD)-based inclusion complexes of CoFe₂O₄ magnetic nanoparticles (MNPs) were prepared and used as catalysts for chemiluminescence (CL) system using the luminol-hydrogen peroxide CL reaction as a model. The as-prepared inclusion complexes were characterized by XRD (X-ray diffraction), TGA (thermal gravimetric analysis) and FT-IR. The oxidation reaction between luminol and hydrogen peroxide in basic media initiated CL. The effect of β−CD-based inclusion complexes of CoFe₂O₄ magnetic nanoparticles and naked CoFe₂O₄ magnetic nanoparticles on the luminol-hydrogen peroxide CL system was investigated. It was found that inclusion complexes between β−CD and CoFe₂O₄ magnetic nanoparticles could greatly enhance the CL of the luminol-hydrogen peroxide system. Investigation on the kinetic curves and the chemiluminescence spectra of the luminol-hydrogen peroxide system demonstrates that addition of CoFe₂O₄ MNPs or inclusion complexes between β−CD and CoFe₂O₄ MNPs does not produce a new luminophor of the chemiluminescent reaction. The luminophor for the CL system was still the excited-state 3-aminophthalate anions (3-APA*). The enhanced CL signals were thus ascribed to the possible catalysis from CoFe₂O₄ MNPs or inclusion complexes between β−CD and CoFe₂O₄ nanoparticles. The feasibility of employing the proposed system for hydrogen peroxide sensing was also investigated. Experimental results showed that the CL emission intensity was linear with hydrogen peroxide concentration in the range of 1.0 × 10⁻⁷ to 4.0 × 10⁻⁶ mol L⁻¹ with a detection limit of 2.0 × 10⁻⁸ mol L⁻¹ under optimized conditions. The proposed method has been used to determine hydrogen peroxide in water samples successfully.     

Molecular imprinted polymer-based chemiluminescence imaging sensor for the detection of trans-resveratrol

Sensitive, rapid and inexpensive chemiluminescence (CL) imaging has been developed based on molecular imprinted polymer (MIP) sensing elements. Imprinted uniform microspheres were synthesized by precipitation polymerization. Microtiter plates (96 wells) were coated with polymer microspheres imprinted with trans-resveratrol, which were fixed in place using poly(vinyl alcohol) (PVA) as glue. The amount of polymer-bound trans-resveratrol was quantified using imidazole (IMZ)-catalyzed peroxyoxalate chemiluminescence (PO-CL) reaction. The light produced was then measured with a high-resolution CCD camera. Calibration curve corresponding to analyte concentration ranging from 0.3 to 25 μg mL⁻¹ was obtained with a limit of detection 0.1 μg mL⁻¹. These results showed that the MIP-based CL imaging sensor can become a useful analytical tool for quick simultaneous detection of trans-resveratrol in a large number of real samples.     

Investigation on enhanced chemiluminescence reaction systems with bis(hydrogenperiodato) argentate(III) complex anion for fluoroquinolones synthetic antibiotics

A novel chemiluminescence (CL) reaction system with bis(hydrogenperiodato) argentate(III) complex anion (Ag(III) complex, [Ag(HIO₆)₂]⁵⁻), for the first time, is developed for the determination of lomefloxacin (LMFX), enrofloxacin (ENLX) and pefloxacin (PFLX). The possible CL emission mechanism was discussed by comparing the fluorescence emission with CL spectra. The CL conditions of [Ag(HIO₆)₂]⁵⁻-H₂SO₄-LMFX/ENLX/PFLX systems were investigated and optimized. Under the optimized experimental conditions, the CL intensity is proportional to the concentration of the drugs in the range 0.2994-36.80 × 10⁻⁷ g mL⁻¹ for LMFX, 4.00-30.0 × 10⁻⁷ g mL⁻¹ for ENLX and 1.54-27.64 × 10⁻⁷ g mL⁻¹ for PFLX. The limit of detection (s/n = 3) was 9.1 × 10⁻⁹ g mL⁻¹ for LMFX, 3.1 × 10⁻⁹ g mL⁻¹ for ENLX and 4.4 × 10⁻⁹ g mL⁻¹ for PFLX. The recovery of LMFX, ENLX and PELX from the spiked pharmaceutical preparations was in the range of 92.3-105% with the RSDs of 0.5-2.7%. For urine, serum and milk samples the recoveries of the three drugs were in the range of 85.1-107% for LMFX with the RSDs of 2.3-3.4%. 80.2-112% for ENLX with the RSDs of 1.4-2.8%, and 87.8-114% for PFLX with the RSDs of 1.6-2.7%. The proposed method was applied successfully to the determination of these compounds in real samples.     

Determination of itopride hydrochloride by high-performance liquid chromatography with Ru(bpy)3 electrogenerated chemiluminescence detection

In this work, a stable electrogenerated chemiluminescence (ECL) detector was developed. The detector was prepared by packing cation-exchanged resin particles in a glass tube, followed by inserting Pt wires (working electrode) in this tube and sealing. The leakage of Ru(bpy)₃²⁺ can be compensated by adding a small amount of Ru(bpy)₃²⁺ into solution phase. Coupled with high-performance liquid chromatography separation, the detector has been used for determination of itopride hydrochloride in human serum. Under the optimal conditions, the ECL intensity has a linear relationship with the concentration of itopride hydrochloride in the range of 1.0 × 10⁻⁸ g mL⁻¹ to 1.0 × 10⁻⁶ g mL⁻¹ and the detection limit was 3 × 10⁻⁹ g mL⁻¹ (S/N = 3). The as-prepared ECL detector displayed good sensitivity and stability.     

A cataluminescence gas sensor based on nanosized V2O5 for tert-butyl mercaptan

This work proposed a gas sensor for the determination of tert-butyl mercaptan, one of the highly toxic volatile sulfur compounds, which was based on cataluminescence emission during its catalytic oxidation on the surface of nanosized V₂O₅. The cataluminescence characteristics and the optimum conditions, including the morphology of sensing material, the wavelength of cataluminescence emission, the oxygen flow rate and working temperature were investigated in detail. Under the optimized conditions, the calibration curve of the relative cataluminescence intensity versus the concentration of tert-butyl mercaptan vapor was made, with the linear range of 5.6-196 μg mL⁻¹ and the detection limit of 0.5 μg mL⁻¹ (S/N = 3). The relative standard deviation (R.S.D.) (n = 5) of relative cataluminescence intensity for 84 μg mL⁻¹ tert-butyl mercaptan was 3.6%. There is no or weak response to some common substances, such as formic acid, alcohol (methanol, ethanol, propanol, isopropanol, n-butanol, isoamyl alcohol), o-dichlorobenzene, acetonitrile, ethyl acetate, aldehyde (formaldehyde, acetaldehyde and propanal), 1,2-dichloroethane and ammonia. Furthermore, the proposed sensor was successfully used for determining tert-butyl mercaptan in four artificial samples, with a good recovery. The results demonstrated that the proposed gas sensor had a promising capability for the tert-butyl mercaptan in routine monitoring.     

Sub-picogram determination of Vitamin B12 in pharmaceuticals and human serum using flow injection with chemiluminescence detection

A sensitive chemiluminescence (CL) method, based on the enhancive effect of cobalt(II) on the CL reaction between luminol and dissolved oxygen in a flow injection (FI) system, was proposed for determination of Vitamin B₁₂. The increment of the CL intensity was proportional to the concentration of Vitamin B₁₂, giving a calibration graph linear over the concentration from 2.0×10⁻¹⁰ to 1.2×10⁻⁶ g l⁻¹ (r²=0.9992) with the detection limit of 5.0×10⁻¹¹ g l⁻¹ (3σ). At a flow rate of 2.0 ml min⁻¹, a complete determination of Vitamin B₁₂, including sampling and washing, could be accomplished in 0.5 min with the relative standard deviations (R.S.D.) of less than 5.0%. The proposed method was applied successfully to the determination of Vitamin B₁₂ in pharmaceuticals, human serum, egg yolk and fish tissue.     

A chitosan–polypyrrole magnetic nanocomposite as μ-sorbent for isolation of naproxen

An extracting medium based on chitosan–polypyrrole (CS–PPy) magnetic nanocomposite was synthesized by chemical polymerization of pyrrole at the presence of chitosan magnetic nanoparticles (CS-MNPs) for micro-solid phase extraction. In this work, magnetic nanoparticles, the modified CS-MNPs and different types of CS–PPy magnetic nanocomposites were synthesized. Extraction efficiency of the CS–PPy magnetic nanocomposite was compared with the CS-MNPs and Fe₃O₄ nanoparticles for the determination of naproxen in aqueous samples, via quantification by spectrofluorimetry. The scanning electron microscopy images obtained from all the prepared nanocomposites revealed that the CS–PPy magnetic nanocomposite possess more porous structure. Among different synthesized magnetic nanocomposites, CS–PPy magnetic nanocomposite showed a prominent efficiency. Influencing parameters on the morphology of CS–PPy magnetic nanocomposite such as weight ratio of components was also assayed. In addition, effects of different parameters influencing the extraction efficiency of naproxen including desorption solvent, desorption time, amount of sorbent, ionic strength, sample pH and extraction time were investigated and optimized. Under the optimum condition, a linear calibration curve in the range of 0.04–10 μg mL⁻¹ (R² = 0.9996) was obtained. The limits of detection (3S_b) and limits of quantification (10S_b) of the method were 0.015 and 0.04 μg mL⁻¹ (n = 3), respectively. The relative standard deviation for water sample spiked with 0.1 μg mL⁻¹ of naproxen was 3% (n = 5) and the absolute recovery was 92%. The applicability of method was extended to the determination of naproxen in tap water, human urine and plasma samples. The relative recovery percentages for these samples were in the range of 56–99%.     

A cataluminescence gas sensor for carbon tetrachloride based on nanosized ZnS

A novel and sensitive gas sensor was proposed for the determination of carbon tetrachloride based on its cataluminescence (CTL) by oxidation in the air on the surface of nanosized ZnS. The luminescence characteristics and the optimal conditions were investigated in detail. Under the optimized conditions, the linear range of the CTL intensity versus the concentration of carbon tetrachloride was 0.4-114 μg mL⁻¹, with a correlation coefficient (R) of 0.9986 and a limit of detection (S/N = 3) of 0.2 μg mL⁻¹. The relative standard deviation (R.S.D.) for 5.9 μg mL⁻¹ carbon tetrachloride was 2.9% (n = 5). There was no or weak response to common foreign substances including methanol, ethanol, benzene, acetone, formaldehyde, acetaldehyde, dichloromethane, xylene, ammonia and trichloromethane. There was no significant change of the catalytic activity of the sensor for 40 h over 4 days, with a R.S.D. of less than 5% by collecting the CTL intensity once an hour. The proposed method was simple and sensitive, with a potential of detecting carbon tetrachloride in environment and industry grounds. The possible mechanism was also discussed briefly.     

Quenched electrochemiluminescence of Ag nanoparticles functionalized g-C3N4 by ferrocene for highly sensitive immunosensing

In this paper, a novel sandwich electrochemiluminescence (ECL) immunosensor was constructed by ferrocene for quenching Ag nanoparticles functionalized g-C₃N₄ (Ag@g-C₃N₄) emission. The prepared Ag@g-C₃N₄ had strong and stable ECL signals compared to pure g-C₃N₄ and primary antibody (Ab₁) can be immobilized on Ag@g-C₃N₄ by adsorption of Ag nanoparticles. Ferrocene carboxylic acid (Fc-COOH) labeled secondary antibody was immobilized on Au doped mesoporous Al₂O₃ nanorods (Au@Al₂O₃–Fc-COOH@Ab₂) as labels through adsorption ability of Au toward proteins. After a sandwich-type immunoreaction, a remarkable decrease of ECL signal was observed due to the ECL quenching of Ag@g-C₃N₄ by Au@Al₂O₃–Fc-COOH@Ab₂. As a result, the change of ECL intensity has a direct relationship with the logarithm of CEA concentrations in the range of 1 pg mL⁻¹–100 ng mL⁻¹ with a detection limit of 0.35 pg mL⁻¹ (S/N = 3). Additionally, the proposed immunosensor shows high specificity, good reproducibility, and long-term stability.     

Simultaneous chemiluminescence determination of promazine and fluphenazine using support vector regression

In this work, chemiluminescence (CL) behaviors of two selected phenothiazines, namely promazine and fluphenazine hydrochloride, were investigated for their simultaneous determination using oxidation of Ru(bipy)₃²⁺ by Ce⁴⁺ ions in acidic media. This method is based on the kinetic distinction of the CL reactions of fluphenazine and promazine with Ru(bipy)₃²⁺ and Ce⁴⁺ system in a sulfuric acid medium. Least square support vector regression models were constructed for relating concentrations of both compounds to their CL profiles. The parameters of the model consisting of σ² and γ were optimized using all possible combinations of σ² and γ to select the model with the minimum root mean square cross validation. Under optimized conditions, the univariate calibration curve was linear over the concentration ranges of 0.4-30.0 μg mL⁻¹ and 0.07-5.0 μg mL⁻¹ with detection limits of 0.1 μg mL⁻¹ and 0.04 μg mL⁻¹ for promazine and fluphenazine, respectively. The influence of potential interfering substances on the determination of promazine and fluphenazine were studied. The proposed method was used for simultaneous determination of both compounds in synthetic mixtures and in spiked human plasma.     

High-pressure transitions in MgAl2O4 and a new high-pressure phase of Mg2Al2O5

Phase transitions in MgAl₂O₄ were examined at 21-27 GPa and 1400-2500 °C using a multianvil apparatus. A mixture of MgO and Al₂O₃ corundum that are high-pressure dissociation products of MgAl₂O₄ spinel combines into calcium-ferrite type MgAl₂O₄ at 26-27 GPa and 1400-2000 °C. At temperature above 2000 °C at pressure below 25.5 GPa, a mixture of Al₂O₃ corundum and a new phase with Mg₂Al₂O₅ composition is stable. The transition boundary between the two fields has a strongly negative pressure-temperature slope. Structure analysis and Rietveld refinement on the basis of the powder X-ray diffraction profile of the Mg₂Al₂O₅ phase indicated that the phase represented a new structure type with orthorhombic symmetry (Pbam), and the lattice parameters were determined as a=9.3710(6) Å, b=12.1952(6) Å, c=2.7916(2) Å, V=319.03(3) Å³, Z=4. The structure consists of edge-sharing and corner-sharing (Mg, Al)O₆ octahedra, and contains chains of edge-sharing octahedra running along the c-axis. A part of Mg atoms are accommodated in six-coordinated trigonal prism sites in tunnels surrounded by the chains of edge-sharing (Mg, Al)O₆ octahedra. The structure is related with that of ludwigite (Mg, Fe²⁺)₂(Fe³⁺, Al)(BO₃)O₂. The molar volume of the Mg₂Al₂O₅ phase is smaller by 0.18% than sum of molar volumes of 2MgO and Al₂O₃ corundum. High-pressure dissociation to the mixture of corundum-type phase and the phase with ludwigite-related structure has been found only in MgAl₂O₄ among various A²⁺B³⁺₂O₄ compounds.     

A novel magnetic poly(aniline-naphthylamine)-based nanocomposite for micro solid phase extraction of rhodamine B

A novel Fe₃O₄–poly(aniline-naphthylamine)-based nanocomposite was synthesized by chemical oxidative polymerization process as a magnetic sorbent for micro solid phase extraction. The scanning electron microscopy images of the synthesized nanocomposite revealed that the copolymer posses a porous structure with diameters less than 50 nm. The extraction efficiency of this sorbent was examined by isolation of rhodamine B, a mutagenic and carcinogenic dye, from aquatic media in dispersion mode. Among different synthesized polymers, Fe₃O₄/poly(aniline-naphthylamine) nanocomposite showed a prominent efficiency. Parameters including the desorption solvent, amount of sorbent, desorption time, sample pH, ionic strength, extraction time and stirring rate were optimized. Under the optimum condition, a linear spiked calibration curve in the range of 0.35–5.00 μg L⁻¹ with R² = 0.9991 was obtained. The limits of detection (3S_b) and limits of quantification (10S_b) of the method were 0.10 μg L⁻¹ and 0.35 μg L⁻¹ (n = 3), respectively. The relative standard deviation for water sample with 0.5 μg L⁻¹ of RhB was 4.2% (n = 5) and the absolute recovery was 92%. The method was applied for the determination of rhodamine B in dishwashing foam, dishwashing liquid, shampoo, pencil, matches tips and eye shadows samples and the relative recovery percentage were in the range of 94–99%.     

Speciation of selenomethionine and selenocystine using online micro-column containing Cu(II) loaded nanometer-sized Al2O3 coupled with ICP-MS detection

A flow injection online speciation procedure by using micro-column packed with Cu(II) loaded nanometer-sized Al₂O₃ coupled to inductively coupled plasma mass spectrometry (ICP-MS) for the separation and determination of selenomethionine (SeMet) and selenocystine (SeCys₂) has been developed. The main factors affecting the separation and preconcentration of SeMet and SeCys₂ including pH value, sample flow rate, eluent concentration, eluent volume and flow rate, and interfering ions have been investigated. It was found that SeCys₂ could be selectively retained by micro-column packed with Cu(II) loaded nanometer-sized Al₂O₃ at pH 4.0, and the retained SeCys₂ could be eluted by 1.0 mol L⁻¹ HNO₃, while SeMet was not retained and passed through the micro-column directly at this pH. Both SeMet and SeCys₂ could be quantitatively adsorbed by the micro-column at pH 9.0, and the retained SeMet and SeCys₂ could be easily eluted with 1.0 mol L⁻¹ HNO₃. The content of SeMet was obtained by subtracting the SeCys₂ from the total content of seleno amino acids. With the enrichment factor of 7.8 and 7.7, the limits of detection (LODs) for SeMet and SeCys₂ were found to be 24 pg Se mL⁻¹ and 21 pg Se mL⁻¹, respectively. The relative standard deviations (RSDs) for SeCys₂ and SeMet with seven replicate determinations of 1.0 ng mL⁻¹ SeMet and SeCys₂, were 2.1% and 1.6%, respectively, the sampling frequency of 8 h⁻¹ was obtained. The proposed method was applied to the speciation of SeMet and SeCys₂ in selenized yeast, human urine and serum with satisfactory results.     

Determination of ketotifen by using calcein as chemiluminescence reagent

Chemiluminescence (CL) was observed when potassium hexacyanoferrate(III) reacted with the mixture of calcein and ketotifen. Interestingly, the CL intensity would be enhanced by trace amounts of Mg²⁺ and the CL intensity was strongly dependent on ketotifen concentration. Based on this phenomenon, a flow injection CL method was established for the determination of ketotifen. The possible CL mechanism is proposed based on the kinetic characteristic of the CL reaction, CL spectrum, ultraviolet (UV) spectra and fluorescent spectra. The CL intensity was correlated linearly with concentration of ketotifen over the range of 6.0 × 10⁻⁹ to 2.0 × 10⁻⁷ g mL⁻¹ and the detection limit was 3 × 10⁻⁹ g mL⁻¹. The relative standard deviation was 1.8% for 2.0 × 10⁻⁸ g mL⁻¹ ketotifen (n = 11). This method was applied to the determination of ketotifen in the tablets successfully.     

A highly sensitive coupling technique for the determination of trace quercetin based on solid substrate room temperature phosphorimetry and poly (vinyl alcohol) complex imprinting

Al³⁺ could react with quercetin (Q) to form [AlQ]³⁺ complex which could be used as a template for the preparation of poly (vinyl alcohol)–[AlQ]³⁺ complex imprinting (PVA-C-I). The [AlQ]³⁺ not only had good matching ability and selectivity with the cavity of PVA-C-I, but also could react with the fluorescein isothiocyanate anion (FITC⁻) on the outside of cavity by electrostatic interaction to form ion-association complex [AlQ]³⁺·[(FITC)⁻]₃. The ion-association complex could emit strong and stable room temperature phosphorescence (RTP) on polyamide membrane (PAM) and the ΔI_p of the system had linear relationship with the content of Q, showing the highly selective identification of PVA-C-I to Q. Thus, a new coupling technique for the determination of trace Q based on solid substrate room temperature phosphorimetry and poly (vinyl alcohol) complex imprinting (PVA-C-I-SSRTP) was established. The linear range and limit of detection (LOD) of this method were 0.010–2.0 (×10⁻¹² g mL⁻¹) and 2.0 × 10⁻¹⁴ g mL⁻¹, respectively, showing wide linear range and high sensitivity of PVA-C-I-SSRTP. This method was used to determine the content of Q in waste water, and the results are consistent with those by spectrofluorimetry. Meanwhile, the mechanism for the determination of Q using PVA-C-I-SSRTP was also discussed.     

Determination of beta-lactam antibiotics in milk using micro-flow chemiluminescence system with on-line solid phase extraction

In this paper, a chemiluminescence (CL) micro-flow system combined with on-line solid phase extraction (SPE) is presented for determination of β-lactam antibiotics (penicillin, cefradine, cefadroxil, cefalexin) in milk. It is based on the enhancement effect of β-lactam antibiotics on the luminol-K₃Fe(CN)₆ CL system. The micro-flow system was fabricated from two polymethyl methacrylate (PMMA) plates (50 mm × 40 mm × 5 mm) with the microchannels of 200 μm wide and 150 μm deep. C₁₈-modified silica gel was packed into the microchannel (length: 10 mm; width: 1 mm; depth: 500 μm) to serve as SPE device. Extraction and preconcentration of the analytes were carried out using on-line SPE micro-flow system and the selectivity of CL detection was improved. The detection limits were 0.5 μg mL⁻¹ of penicillin, 0.04 μg mL⁻¹ of cefradine, 0.08 μg mL⁻¹ of cefadroxil and 0.1 μg mL⁻¹ of cefalexin. The proposed method was also applied to analyze the β-lactam antibiotics in milk. Experimental results were in good agreement with those obtained by high performance liquid chromatography (HPLC) method with UV detection.     

Flow-injection post chemiluminescence determination of atropine sulfate

A new post chemiluminescence (PCL) reaction was observed when atropine sulfate was injected into the reaction mixture after the finish of CL reaction of Ce(IV) and sodium sulfite. The possible mechanism for the PCL reaction was discussed via the investigation of the CL kinetic characteristics, the CL spectra, the UV absorption spectra and the fluorescence spectra of some related substances. The flow injection PCL method for the determination of atropine sulfate was established. The relative standard deviation (R.S.D.) was 2.8% (n = 11, c = 5.0 × 10⁻⁶ g mL⁻¹). The PCL intensity responded linearly to the concentration of atropine sulfate in the range 1.0 × 10⁻⁶ to 5.0 × 10⁻⁵ g mL⁻¹ with a linear correlation of 0.9947. The detection limit was 4 × 10⁻⁷ g mL⁻¹ atropine sulfate. The method had been applied to the determination of atropine sulfate in the tablets and the results were consistent with the method of Chinese pharmacopoeia.