A quick method for the simultaneous determination of ascorbic acid and sorbic acid in fruit juices by capillary zone electrophoresis

A method of quickly determining ascorbic acid and sorbic acid by capillary zone electrophoresis with ultraviolet detection was developed. The choice of background electrolyte, wavelength, injection time and applied voltage were discussed. Ascorbic acid and sorbic acid were well separated in 80 mmol L⁻¹ boric acid-5 mmol L⁻¹borax (pH = 8.0) in 5 min at the detecting wavelength of 270 nm. Under the optimum condition, the method has linear ranges of 2.54-352.00 mg L⁻¹ for ascorbic acid and 1.08-336.39 mg L⁻¹ for sorbic acid with the detection limit of 1.70 mg L⁻¹ for ascorbic acid and 0.54 mg L⁻¹ for sorbic acid, respectively. Other organic acids in fruit juices have no effect on the detection. This method is very feasible and simple and can be used to detect ascorbic acid and sorbic acid in fruit juices.     

Sample cleanup-free determination of mycophenolic acid and its glucuronide in serum and plasma using the novel technology of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry

Mycophenolic acid (MPA) is an immunosuppressant drug which powerfully inhibits lymphocyte proliferation. Since the early 1990s it has been used to prevent rejection in organ transplantation. The requirement of therapeutic drug monitoring shown in previous studies raises the necessity of acquiring accurate and sensitive methods to measure MPA and its major metabolite mycophenolic acid glucuronide (MPAG).The authors developed a sample cleanup-free, rapid, and highly specific method for simultaneous measurement of MPA and MPAG in human plasma and serum using the novel technology of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry. MPA- and MPAG-determinations were performed during a 2.0-min run time. Multiple calibration curves for the analysis of MPA and MPAG exhibited consistent linearity and reproducibility in the range of 0.05-100 (r > 0.999) mg L⁻¹ and 4-4000 mg L⁻¹ (r > 0.999), respectively. Limits of Detection were 0.014 mg L⁻¹ for MPA and 1.85 mg L⁻¹ for MPAG. Lower Limits of Quantification were 0.05 mg L⁻¹ for MPA and 2.30 mg L⁻¹ for MPAG. Interassay imprecision was <10% for both substances. Mean recovery was 103.6% (range 78.1-129.7%) for MPA and 111.1% (range 73.0-139.6%) for MPAG. Agreement was good for MPA and MPAG between the presented method and a validated HPLC-MS/MS method. The Passing-Bablok regression line for MPA and MPAG was HPLC-MS/MS = 1.14 UPLC-MS/MS—0.14 [mg L⁻¹], r = 0.96, and HPLC-MS/MS = 0.77 UPLC-MS/MS + 0.50 [mg L⁻¹], r = 0.97, respectively. This sample cleanup-free and robust LC-MS/MS assay facilitates the rapid, accurate and simultaneous determination of MPA and MPAG in human body fluids.     

Development of method for the speciation of inorganic iron in wine samples

In this paper, we proposed a procedure for the determination of iron(II) and total iron in wine samples employing molecular absorption spectrophotometry. The ligand used is 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol (Br-PADAP) and the chromogenic reaction in absence or presence of ascorbic acid (reducing agent) allows the determination of iron(II) or total iron, respectively. The optimization step was performed using a multivariate technique (Box Behnken design) involving the factors pH, acid ascorbic concentration and reaction time.The method allows the determination of iron(II) and iron(III) in wine samples, with limits of detection and quantification 0.22 and 0.72 μg L⁻¹, respectively. The precision expressed as relative standard deviation (R.S.D.) was 1.43 and 0.56% (both, n = 11) for content of iron(II) in wine samples of 1.68 and 4.65 mg L⁻¹, and 1.66 and 0.87% (both, n = 11) for content of total iron in wine samples of 1.72 and 5.48 mg L⁻¹.This method was applied for determination of iron(II) and total iron in six different wine samples. In these, the iron(II) content varied from 0.76 to 4.65 mg L⁻¹ and from 1.01 to 5.48 mg L⁻¹ for total iron. The results obtained in the determination of total iron by Br-PADAP method were compared with those that were performed after complete acid digestion in open system and determination of total iron employing FAAS. The method of regression linear was used for comparison of these results and demonstrated that there is no significant difference between the results obtained with these two procedures.     

Fluorimetric determination of phytic acid in urine based on replacement reaction

A sensitive fluorimetric method for determination of phytic acid in human urine samples was described. The method was based on a fluorimetric replacement reaction, in which the added phytic acid replaced the Cu²⁺ ion from Cu²⁺-gelatin complex, liberating the fluorescent gelatin molecule. The fluorescence of the solution was accordingly recovered proportionally to the amount of the foreign phytic acid. The excitation wavelength was 273.5 nm and the characteristic emission wavelength was 305.0 nm, respectively. The calibration graph was obtained by plotting the recovered fluorescent intensity at maximum 305.0 nm against the added standard phytic acid, and was divided into two sections. One section was linear over the range of 0.40-2.40 mg L⁻¹ with a linear regression equation of I_f = −0.895 + 15.146c (R² > 0.9993), and the other over the range of 2.40-9.20 mg L⁻¹ with a linear regression equation of I_f = −29.526 + 26.113c (R² > 0.9996), respectively. The relative standard deviation (R.S.D.) at 95% confidence degree for a 2.0 mg L⁻¹ of standard phytic acid within 1 month was less than 1.26% (n = 5), indicating the procedure is reproducible. The detection and the quantification limits of phytic acid were estimated to be 0.23 and 0.40 mg L⁻¹, respectively. The proposed method was applied to the determination of phytic acid in urine samples and the found concentrations of phytic acid in urine were in the range of 0.49-0.75 mg L⁻¹ with recoveries of 96.2-108.8%. Comparison of the obtained results with the reported HPLC was performed, indicating the proposed method was reliable.     

Analysis of potassium formate in airport storm water runoff by headspace solid-phase microextraction and gas chromatography–mass spectrometry

Potassium formate was extracted from airport storm water runoff by headspace solid-phase microextraction (HS-SPME) and analyzed by GC–MS. Formate was transformed to formic acid by adding phosphoric acid. Subsequently, formic acid was derivatized to methyl formate by adding methanol. Using sodium [²H]formate (formate-d) as an internal standard, the relative standard deviation of the peak area ratio of formate (m/z 60) and formate-d (m/z 61) was 0.6% at a concentration of 208.5 mg L⁻¹. Calibration was linear in the range of 0.5–208.5 mg L⁻¹. The detection limit calculated considering the blank value was 0.176 mg L⁻¹. The mean concentration of potassium formate in airport storm water runoff collected after surface de-icing operations was 86.9 mg L⁻¹ (n = 11) with concentrations ranging from 15.1 mg L⁻¹ to 228.6 mg L⁻¹.     

The development of sequential injection analysis coupled with lab-on-valve for copper determination

A sequential injection analysis (SIA) using lab-on-valve with air segmentation and spectrophotometric detection was designed for copper(II) determination. It is based on the reaction of copper(II) and 2-carboxy-2′-hydroxy-5′-sulfoformazyl benzene (Zincon) in a weak alkaline solution between the air zones. Beer's Law was obeyed over the range of 0.1-2.0 mg L⁻¹ copper(II) with a correlation coefficient 0.9985 and a slope of 0.2893 absorbance unit/mg L⁻¹. The relative standard deviation was 2.0% for a series of 10 measurements of 0.5 mg L⁻¹ copper(II) solution. The detection limit (3 S/N) and the limit of quantification (LOQ) were 0.05 and 0.17 mg L⁻¹ respectively. This method has been successfully applied to determination of copper(II) in wastewater with a sample throughput of 120 h⁻¹. The method is superior to the batchwise method in that it provides fully automation, rapidity, less reagents and sample consumption with little waste generation.     

A multicommuted flow system for sequential spectrophotometric determination of hydrosoluble vitamins in pharmaceutical preparations

A multicommuted flow system is proposed for spectrophotometric determination of hydrosoluble vitamins (ascorbic acid, thiamine, riboflavine and pyridoxine) in pharmaceutical preparations. The flow manifold was designed with computer-controlled three-way solenoid valves for independent handling of sample and reagent solutions and a multi-channel spectrophotometer was employed for signal measurements. Periodic re-calibration as well as the standard addition method was implemented by using a single reference solution. Linear responses (r=0.999) were obtained for 0.500-10.0 mg l⁻¹ ascorbic acid, 2.00-50.0 mg l⁻¹ thiamine, 5.00-50.0 mg l⁻¹ riboflavine and 0.500-8.00 mg l⁻¹ pyridoxine. Detection limits were estimated as 0.08 mg l⁻¹ (0.5 μmol l⁻¹) ascorbic acid, 0.8 mg l⁻¹ (2 μmol l⁻¹) thiamine, 0.2 mg l⁻¹ (0.5 μmol l⁻¹) riboflavine and 0.1 mg l⁻¹ (0.9 μmol l⁻¹) pyridoxine at 99.7% confidence level. A mean sampling rate of 60 determinations per hour was achieved and coefficients of variation of 1% (n=20) were estimated for all species. The mean reagent consumption was 25-fold lower in relation to flow-based procedures with continuous reagent addition. Average recoveries between 95.6 and 100% were obtained for commercial pharmaceutical preparations. Results agreed with those obtained by reference methods at 95% confidence level. The flow system is suitable for application in quality control processes and in dissolution studies of vitamin tablets.     

A new method for electrocatalytic oxidation of ascorbic acid at the Cu(II) zeolite-modified electrode

A new method is developed for the catalytic oxidation of ascorbic acid at graphite zeolite-modified electrode, doped with copper(II) (Cu²⁺A/ZCME). Copper(II) exchanged in zeolite type A acts as catalyst to oxidize ascorbic acid. The modified electrode lowered the overpotential of the reaction by ∼400 mV. First, the electrochemical behavior of copper(II), incorporated in the zeolite type A modified electrode, was studied. The results illustrate that diffusion can control the copper(II)/copper(0) redox process at the Cu²⁺A/ZCME. Then, the behavior of electrocatalytic oxidation reaction for ascorbic acid was researched. The electrode was employed to study electrocatalytic oxidation of ascorbic acid, using cyclic voltammetry and chronoamperometry as diagnostic techniques. The diffusion coefficient of ascorbic acid was equal to 1.028 × 10⁻⁵ cm² s⁻¹. A linear calibration graph was obtained over the ascorbic acid with a concentration range of 0.003-6.00 mmol L⁻¹. The detection limit (DL) of ascorbic acid was estimated as 2.76 × 10⁻⁷ mol L⁻¹. The relative standard deviations of 10 replicate measurements (performed on a single electrode at several ascorbic acid concentrations between 3.0 and 200 μmol L⁻¹) were measured between 1.0 and 2.4%.     

A green analytical procedure for flow-injection determination of nitrate in natural waters

Nitrate determination in waters is generally carried out with cadmium filings and carcinogenic reagents or by reaction with phenolic compounds in highly concentrated sulfuric acid medium. In this work, it was developed a green analytical procedure for nitrate determination in natural waters based on direct spectrophotometric measurements in ultraviolet, using a flow-injection system with an anion-exchange column for separation of nitrate from interfering species. The proposed method employs only one reagent (HClO₄) in a minimum amount (equivalent to 18 μL concentrated acid per determination), and allowed nitrate determination within 0.50-25.0 mg L⁻¹, without interference of up to 200.0 mg L⁻¹ humic acid; 1.0 mg L⁻¹ NO₂⁻; 200.0 mg L⁻¹ PO₄³⁻; 75.0 mg L⁻¹ Cl⁻; 50.0 mg L⁻¹ SO₄²⁻ and 15.0 mg L⁻¹ Fe³⁺. The detection limit (99.7% confidence level) and the coefficient of variation (n = 20) were estimated as 0.1 mg L⁻¹ and 0.7%, respectively. The results obtained for natural water samples were in agreement with those achieved by the reference method based on nitrate reduction with copperized cadmium at the 95% confidence level.     

A simple colorimetric FIA method for the determination of pyrite oxidation rates

A method for the rapid determination of the oxidation rate of naturally occurring pyrite (FeS₂) samples is presented. The progress of the oxidation reaction was followed by measurement of the concentration of total dissolved iron using flow injection analysis. Iron was determined using UV-vis detection after reaction with the colorimetric reagent 5-sulfosalicylic acid in the presence of ammonia. The calibration function was linear between 5 and 150 mg L⁻¹, and the detection limit was 0.46 mg L⁻¹. The relative standard deviation was typically less than 1% (n = 10) and the measurement frequency was 60/h. The method was used to quantify the oxidation rate of 10 ground and cleaned pyrite samples (53 μm < x < 106 μm) from various international locations that were subjected to accelerate oxidation in acidic hydrogen peroxide. Results of these experiments showed that there was almost an order of magnitude of difference in oxidation rates of the pyrite samples.     

Direct chiral resolution and its application to the determination of fungicide benalaxyl in soil and water by high-performance liquid chromatography

A simple chiral high-performance liquid chromatography (HPLC) method with ultraviolet (UV) and circular dichroism (CD) detection was developed and validated for measuring benalaxyl enantiomers using (R,R) Whelk-O 1 column. The effects of mobile phase composition and column temperature on the entioseparation were investigated. A CD detector was used to determine the elution order of the enantiomers. Excellent resolution was easily obtained using n-hexane-polar organic alcohols mobile phase. The chiral recognition mechanism was also discussed. Based on the developed chiral HPLC method, enantioselective analysis methods for this fungicide in environment matrix (soil and water) were developed and validated. Good linearities were obtained over the concentration range of 0.25-25 mg L⁻¹ for both enantiomers. Liquid-liquid extraction and solid phase extraction (SPE) were used for the enrichment and cleanup of soil and water samples. Recoveries for the two enantiomers were 79-91% at 0.02, 0.04 and 0.2 mg kg⁻¹ levels from soil, and 89-101% at 0.0025, 0.01 and 0.05 mg L⁻¹ levels from water. Run-to-run and day-to-day assay precisions were below 10% for both enantiomers at concentrations of 0.5, 1 and 5 mg L⁻¹. Individual detection limits of the two enantiomers were both 2 ng. Limits of detection (LOD) were 0.004 mg kg⁻¹ in soil and 0.001 mg L⁻¹ in water.     

Determination of iodide by detection of iodine using gas-diffusion flow injection and chemiluminescence

This work describes development of a flow injection (FI) system for determination of iodide, based on the chemiluminescence (CL) reaction between iodine and luminol. Iodide in the sample zone is oxidized to iodine. Employment of a gas-diffusion (GD) unit allows for selective detection of the generated CL (425 nm). Preliminary results showed for concentrations of less than 2 mg L⁻¹, that signals were irreproducible and that the calibration was not linear.In order to solve these problems, a method of ‘membrane conditioning’ was investigated, in which iodide stream was continuously merged with oxidant to generate I₂ that conditioned the GD membrane and tubing. This minimized surface interaction between the active surface and the I₂ generated from the samples, thus improving both precision and sensitivity. By employing membrane conditioning, it has been possible to reliably detect concentrations down to 0.1 mg L⁻¹.At the optimized condition, an excellent linear calibration (r² = 0.999) was obtained from 0.1 to 1.0 mg L⁻¹. The method was successfully applied to determine iodide in some pharmaceutical products such as potassium iodide tablets and a liquid patent medicine. However, for vitamin tablets, ascorbic acid was found to interfere seriously by causing a negative signal.     

Multivariate optimization and validation of an analytical methodology by RP-HPLC for the determination of losartan potassium in capsules

This paper describes the optimization and validation of an analytical methodology for the determination of losartan potassium in capsules by HPLC using 2^5-1 fractional factorial and Doehlert designs. This multivariate approach allows a considerable improvement in chromatographic performance using fewer experiments, without additional cost for columns or other equipment. The HPLC method utilized potassium phosphate buffer (pH 6.2; 58 mmol L⁻¹)-acetonitrile (65:35, v/v) as the mobile phase, pumped at a flow rate of 1.0 mL min⁻¹. An octylsilane column (100 mm × 4.6 mm i.d., 5 μm) maintained at 35 °C was used as the stationary phase. UV detection was performed at 254 nm. The method was validated according to the ICH guidelines, showing accuracy, precision (intra-day relative standard deviation (R.S.D.) and inter-day R.S.D values <2.0%), selectivity, robustness and linearity (r = 0.9998) over a concentration range from 30 to 70 mg L⁻¹ of losartan potassium. The limits of detection and quantification were 0.114 and 0.420 mg L⁻¹, respectively. The validated method may be used to quantify losartan potassium in capsules and to determine the stability of this drug.     

Selective stopped-flow sequential injection method for the spectrophotometric determination of titanium in dental implant and natural Moroccan phosphate rock

The present work reports the first sequential injection (SI) method for the spectrophotometric determination of Ti(IV). The method is based upon the reaction of Ti(IV) with chromotropic acid (CA) in acidic medium to form a water-soluble complex (λ_max = 420 nm). The chemical and instrumental variables of the system that affected the reaction were studied. Selectivity was greatly enhanced using ascorbic acid. A linear calibration graph was obtained in the range 0.2-10.0 mg l⁻¹ Ti(IV) at a sampling frequency of 24 h⁻¹. The precision was satisfactory (s_r = 1.5% at 5.0 mg l⁻¹ Ti(IV), n = 12) and the 3σ limit of detection, c_L, was 0.7 mg l⁻¹ (n = 10). The developed method proved to be adequately selective and was applied successfully to the analysis of real samples (dental implant and natural Moroccan phosphate rock) giving accurate results based on recovery studies (98-105%).     

A multi-pumping flow-based procedure with improved sensitivity for the spectrophotometric determination of acid-dissociable cyanide in natural waters

An analytical procedure with improved sensitivity was developed for cyanide determination in natural waters, exploiting the reaction with the complex of Cu(I) with 2,2′-biquinoline 4,4′-dicarboxylic acid (BCA). The flow system was based on the multi-pumping approach and long pathlength spectrophotometry with a flow cell based on a Teflon AF 2400^® liquid core waveguide was exploited to increase sensitivity. A linear response was achieved from 5 to 200 μg L⁻¹, with coefficient of variation of 1.5% (n = 10). The detection limit and the sampling rate were 2 μg L⁻¹ (99.7% confidence level), and 22 h⁻¹, respectively. Per determination, 48 ng of Cu(II), 5 μg of ascorbic acid and 0.9 μg of BCA were consumed. As high as 100 mg L⁻¹ thiocyanate, nitrite or sulfite did not affect cyanide determination. Sulfide did not interfere at concentrations lower than 40 and 200 μg L⁻¹ before or after sample pretreatment with hydrogen peroxide. The results for natural waters samples agreed with those obtained by a fluorimetric flow-based procedure at the 95% confidence level. The proposed procedure is then a reliable, fast and environmentally friendly alternative for cyanide determination in natural waters.     

Evaluation of alternate lines of Fe for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry

The usefulness of the secondary line at 252.744 nm and the approach of side pixel registration were evaluated for the development of a method for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The influence of side pixel registration on the sensitivity and linearity was investigated by measuring at wings (248.325, 248.323, 248.321, 248.329, and 248.332 nm) of the main line for Fe at 248.327 nm. For the secondary line at 252.744 nm or side pixel registration at 248.325 nm, main lines for Cu (324.754 nm), Mn (279.482 nm) and Zn (213.875 nm), sample flow-rate of 5.0 mL min⁻¹ and calibration by matrix matching, analytical curves in the 0.2-1.0 mg L⁻¹ Cu, 1.0-20.0 mg L⁻¹ Fe, 0.2-2.0 mg L⁻¹ Mn, 0.1-1.0 mg L⁻¹ Zn ranges were obtained with linear correlations better than 0.998. The proposed method was applied to seven soil samples and two soil reference materials (IAC 277; IAC 280). Results were in agreement at a 95% confidence level (paired t-test) with reference values. Recoveries of analytes added to soil extracts containing 0.15 and 0.30 mg L⁻¹ Cu, 7.0 and 14 mg L⁻¹ Fe, 0.60 and 1.20 mg L⁻¹ Mn, 0.07 and 0.15 mg L⁻¹ Zn, varied within the 94-99, 92-98, 93-101, and 93-103% intervals, respectively. The relative standard deviations (n = 12) were 2.7% (Cu), 1.4% (Fe - 252.744 nm), 5.7% (Fe - 248.325 nm), 3.2% (Mn) and 2.8% (Zn) for an extract containing 0.35 mg L⁻¹ Cu, 14 mg L⁻¹ Fe, 1.1 mg L⁻¹ Mn and 0.12 mg L⁻¹ Zn. Detection limits were 5.4 μg L⁻¹ Cu, 55 μg L⁻¹ Fe (252.744 nm), 147 μg L⁻¹ Fe (248.325 nm), 3.0 μg L⁻¹ Mn and 4.2 μg L⁻¹ Zn.     

Flow injection fluorometric determination of ascorbic acid using perylenebisimide-linked nitroxide

A simple and sensitive flow injection fluorometric method for the determination of ascorbic acid is described. Perylenebisimide-linked nitroxide (PBILN) is used as a fluorescent reagent, which permits the selective determination of ascorbic acid. The fluorescence of the perylenebisimide moiety in PBILN is quenched by the nitroxide moiety, which is linked to the perylenebisimide. When a stream of a solution of ascorbic acid is merged with a stream of PBILN, the ascorbic acid reacts with the nitroxide moiety of PBILN to form hydroxylamine, and the fluorescence properties of the perylenebisimide moiety are recovered. As a result, a peak-shaped fluorescence signal is produced, which can be observed by a fluorescence detector located downstream. Under optimized conditions, a good linear relationship between the concentration of ascorbic acid and peak height in the concentration range from 0.5 to 10 μmol L⁻¹ was found and the detection limit (S/N = 3) was 0.28 μmol L⁻¹. The relative standard deviation for the determination of 4.0 μmol L⁻¹ ascorbic acid samples was 1.0% (n = 5). The proposed method was applied to the determination of ascorbic acid in several soft drink beverages and the analytical results were in good agreement with those obtained using a conventional method.     

A novel, environmentally friendly dispersive liquid-liquid microextraction procedure for the determination of copper

A novel, simple and environmentally friendly procedure for copper determination has been developed. The method is based on the formation of an ion associate of Cu(I) with 1,3,3-trimethyl-2-[5-(1,3,3-trimethyl-1,3-dihydroindol-2-ylidene)-penta-1,3-dienyl]-3H-indolium (DIDC) in the presence of chloride ions as ligand, followed by dispersive liquid-liquid microextraction (DLLME) of the formed ion associate into organic phase and UV-Vis spectrophotometric detection. The following experimental conditions were used: pH 3, 0.24 mol L^− 1 chloride ions, 0.06 mmol L^− 1 DIDC. The effect of the nature of the extraction solvent, auxiliary solvent and disperser solvent used was studied. A mixture of amyl acetate, tetrachloromethane, and methanol in a 1:1:3 v/v/v ratio was selected for the DLLME procedure. The absorbance of the coloured extracts at 640 nm wavelength obeys Beer's law in the range 0.020-0.090 mg L^− 1 of Cu. The limit of detection calculated from a blank test (n = 10) based on 3s is 0.005 mg L^− 1 of Cu. The developed procedure was applied to the analysis of water samples. The suggested DLLME is compared with two procedures previously reported from our laboratory based on (1) conventional liquid-liquid extraction, and (2) sequential injection extraction performed in a dual-valve sequential injection system. The advantages and disadvantages of each method are discussed.     

Simultaneous determination of some food additives in soft drinks and other liquid foods by flow injection on-line dialysis coupled to high performance liquid chromatography

Flow injection on-line dialysis was developed for sample pretreatment prior to the simultaneous determination of some food additives by high performance liquid chromatography (FID-HPLC). A liquid sample or mixed standard solution (900 μL) was injected into a donor stream (5%, w/v, sucrose) of FID system and was pushed further through a dialysis cell, while an acceptor solution (0.025 mol L⁻¹ phosphate buffer, pH 3.75) was held in the opposite side of the dialysis membrane. The dialysate was then flowed to an injection loop of the HPLC valve, where it was further injected into the HPLC system and analyzed under isocratic reverse-phase HPLC conditions and UV detection (230 nm). The order of elution of five food additives was acesulfame-K, saccharin, caffeine, benzoic acid and sorbic acid, respectively, with the analysis time of 14 min. On-line dialysis and HPLC analysis could be performed in parallel, providing sample throughput of 4.3 h⁻¹. Dialysis efficiencies of five food additives were in ranges of 5-11%. Linear calibration graphs were in ranges of 10-100 mg L⁻¹ for acesulfame-K and saccharin, 10-250 mg L⁻¹ for benzoic acid and 10-500 mg L⁻¹ for caffeine and sorbic acid. Good precisions (RSD < 5%) for all the additives were obtained. The proposed system was applied to soft drink and other liquid food samples. Acceptable percentage recoveries could be obtained by appropriate dilution of the sample before injecting into the system. The developed system has advantages of high degrees of automation for sample pretreatment, i.e., on-line sample separation and dilution and low consumption of chemicals and materials.     

Simultaneous determination of eleven quinolones in animal feed by liquid chromatography with fluorescence and ultraviolet absorbance detection

A rapid and simple multi-residue procedure is described for assaying eleven quinolones (cinoxacin, ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, nalidixic acid, norfloxacin, oxolinic acid and sarafloxacin) in feeds at sub-additive levels (1–5 mg kg⁻¹). Five grams of sample were extracted by a metaphosphoric acid/acetonitrile mixture (70/30, v/v) and purified onto OASIS HLB cartridges. The determination was achieved by liquid chromatography (LC) using a GEMINI C18 analytical column both with fluorescence detection (FD) and photodiode-array (DAD). Limits of detection for each drug were in the range 0.04–0.8 mg kg⁻¹. Above the limit of quantification (LOQ), in poultry feed the recoveries were from 69 to 98% with relative standard deviations less than or equal 10%. Finally the measurement uncertainty was estimated using the bottom-up approach.