Rapid spectrophotometric method to resolve ternary mixtures of Tartrazine, Quinoline Yellow and Patent Blue V in commercial products

A very simple spectrophotometric method is described for resolving ternary mixtures of the food dyes Tartrazine (E-102), Quinoline Yellow (E-104) and Patent Blue V (E-131) by using the second derivative of the spectra with measurements at zero-crossing wavelengths. Calibration graphs are linear up to 20.0 mg/L of Tartrazine, up to 20.0 mg/L of Quinoline Yellow and up to 6.4 mg/L of Patent Blue V. Repeatability and reproducibility studies (with the Students’s and F tests) were achieved for two series of nine standards for each dye showing no significant differences at the 95% confidence level. Detection limits of 0.0526, 0.0164 and 0.0034 mg/L were obtained for Tartrazine, Quinoline Yellow and Patent Blue V, respectively. This method was used for determining synthetic mixtures of these colorants in different ratios and it was successfully applied to four commercial products without previous separation step. The results found in commercial products were compared with those obtained by an HPLC method and very similar values were found for both methods.     

Derivative spectrophotometric resolution of mixtures of the food colourants Tartrazine, Amaranth and Curcumin in a micellar medium

A study of the absorption spectra of the food colourants Tartrazine (E-102), Amaranth (E-123) and Curcumin (E-100) in various organic solvents and pH media, have been carried out. In addition, the spectral behaviour in aqueous micellar systems of anionic, cationic and non-ionic surfactants, as well as beta-cyclodextrin, was investigated. Analytical methods are proposed for the determination of the three dyes in mixtures without any prior separation step, by the application of the derivative technique to the normal absorption spectra, based on the use of cetyltrimethylammonium bromide (CTAB) in 0.1 M NaOH, over the concentration range 2-50 mug ml(-1). The methods are applied for determining the three dyes in commercial food products.     

Rapid spectrophotometric method to resolve ternary mixtures of Tartrazine, Quinoline Yellow and Patent Blue V in commercial products

A very simple spectrophotometric method is described for resolving ternary mixtures of the food dyes Tartrazine (E-102), Quinoline Yellow (E-104) and Patent Blue V (E-131) by using the second derivative of the spectra with measurements at zero-crossing wavelengths. Calibration graphs are linear up to 20.0 mg/L of Tartrazine, up to 20.0 mg/L of Quinoline Yellow and up to 6.4 mg/L of Patent Blue V. Repeatability and reproducibility studies (with the Students’s and F tests) were achieved for two series of nine standards for each dye showing no significant differences at the 95% confidence level. Detection limits of 0.0526, 0.0164 and 0.0034 mg/L were obtained for Tartrazine, Quinoline Yellow and Patent Blue V, respectively. This method was used for determining synthetic mixtures of these colorants in different ratios and it was successfully applied to four commercial products without previous separation step. The results found in commercial products were compared with those obtained by an HPLC method and very similar values were found for both methods. Received: 28 December / Revised: 26 May 1999 / Accepted: 31 May 1999     

Simultaneous spectrophotometric determination of three food dyes by using the first derivative of ratio spectra

Ternary mixtures of colorants E-123 (Amaranth), E-124 (Ponceau 4R) and E-120 (Carminic acid) are resolved by using the first derivative ratio spectrum-zero crossing method without the need for any separation step. Calibration graphs were linear up to 64 mg l⁻¹ of carminic acid, 32 mg l⁻¹ of Amaranth and 32 mg l⁻¹ of Ponceau 4R. The method was applied to different commercial food products and results concordant with high performance liquid chromatography were obtained.     

Resolution of ternary mixtures of Tartrazine, Sunset yellow and Ponceau 4R by derivative spectrophotometric ratio spectrum-zero crossing method in commercial foods

A very simple spectrophotometric method is described for resolving ternary mixtures of the food colorants Tartrazine, Sunset Yellow and Ponceau 4R by using the first derivative of the ratio spectra with measurements at zero-crossing wavelengths. Calibration graphs are linear up to 20 mg l(-1) of Tartrazine (E-102), 40 mg l(-1) of Sunset Yellow (E-110) and 32 mg l(-1) of Ponceau 4R (E-124). Standard deviations of 0.9, 0.8 and 2.4% were obtained for nine standards of 8 mg l(-1) of Tartrazine, 8 mg l(-1) of Sunset Yellow and 8 mg l(-1) of Ponceau 4R, respectively. This method was satisfactorily used for determining synthetic mixtures of these colorants in different ratios (from 1:1:1 to 1:5:5 or even higher) with recoveries in 94-105% range and it was successfully applied over three commercial products containing the three dyes and it did not require any separation step. The results were compared with those obtained by HPLC and very similar values were found by both methods.     

Spectrophotometric Simultaneous Determination of Amaranth,Ponceau 4R,Allura Red and Red 2G by Partial Least Squares and Principal Component Regression Multivariate Calibration

ABSTRACT

The multivariate calibration methods, partial least square regression type 1 (PLS 1) and principal component regression (PCR), were proposed for the simultaneous spectrophotometry determination of Amaranth (E-123), Ponceau 4R (E-124), Allura red (E-129) and Red 2G (E-128) in their mixtures. The parameters of the chemometric procedures were optimized and the proposed method was validated with synthetic samples and applied to analyze these dyes in spiked samples of beverages with satisfactory results.     

Development of an HPLC-Method for the Determination of E-2-Nonenal in Beer using Column Switching Techniques

Abstract

E-2-nonenal is an important compound formed during ageing of beer. It has a flavour threshold value of about 0.1 μg/l. A method is described for isolation of E-2-nonenal from beer by solid phase extraction. After extraction E-2-nonenal is derivatized with dansylhydrazine and analyzed with reversed phase HPLC using column switching techniques. The combination of on-line preconcentration of the derivative and heartcutting enables the analysis of E-2-nonenal in beer at natural levels.     

Simultaneous spectrophotometric determination of tartrazine, patent blue V, and indigo carmine in commercial products by partial least squares and principal component regression methods

Two multivariate calibration methods, partial least squares (PLS-1) and principal component regression (PCR) were proposed and successfully applied to the simultaneous determination of three dyes, tartrazine (T) (E-102), patent blue V (P) (E-131), and indigo carmine (I) (E-132) in mixtures by ultraviolet-visible absorption spectrophotometry. Calibration models were evaluated by internal validation (prediction of dyes concentration in its own designed training set of calibration), by cross-validation (obtaining statistical parameters that show the efficiency for a calibration fit model), and by external validation over 19 synthetic mixtures of the three dyes in different ratios containing 2.4-17.6 mg l(-1) of T, 1.6-5.6 mg l(-1) of P, and 3.2-17.5 mg/l(-1) of I, with recoveries between 93.5 and 103.1% and over three commercial products, in which the proposed calibration models were satisfactorily applied without separation step. Repeatability and reproducibility studies (with the Students's and F tests) were achieved over two series of nine standards for each dye, showing no significant differences at 95% confidence level.     

Simultaneous determination of carminic acid, riboflavine, curcumin and erythrosine by derivative spectrophotometry and ratio spectra derivative

A quaternary mixture of carminic acid, riboflavine, curcumin and erythrosine can be resolved with a previous extraction step into metyl-isobutyl ketone and, resolving the binary mixtures obtained in the aqueous phase and organic phase, using derivative spectrophotometry on the basis of the zero-crossing measurements in the first derivative spectra as well as the first derivative of ratio spectra. The conditions of extraction established and the proposed methods have been tested to determine these colorants in several synthetic mixtures of four dyes, obtaining good recoveries. The methods have been applied in yoghurt samples spiked with the dyes.     

Simultaneous spectrophotometric determination of Tartrazine, Sunset Yellow and Ponceau 4R in commercial products by partial least squares and principal component regression multivariate calibration methods

Three multivariate calibration methods, partial least squares (PLS-1 and PLS-2) and principal component regression (PCR), were proposed and successfully applied to the simultaneous determination of three dyes, Tartrazine (E-102), Sunset Yellow (E-110) and Ponceau 4R (E-124) in mixtures by ultraviolet-visible absorption spectrophotometry. The designed and optimized training set of calibration was applied to the determination of the three dyes in several synthetic mixtures, containing 1.6–20.0 mg/L of Tartrazine, 3.2–40.0 mg/L of Sunset Yellow and 3.2– 36.0 mg/L of Ponceau 4R. 94.5–105.3% recovery values were obtained. Three commercial foods that contained the three dyes were also satisfactorily analyzed without separation step. The results obtained by the application of the three chemometric approaches in the commercial products are discussed and compared with those obtained by an HPLC method and very similar values were found by all methods. Repeatability and reproducibility studies (with the Student’s and F tests) were achieved over two series of nine standards for each dye, showing no significant differences at the 95% confidence level.     

High-performance liquid chromatographic determination of a cysteine protease inhibitor and its ethyl ester in mouse serum and muscle by pre-column fluorescence derivatization

A simple and sensitive high-performance liquid chromatographic method has been developed for the determination of a cysteine protease inhibitor (E-64-c) and its ethyl ester in mouse serum and muscle samples. After deproteinization with acetone, E-64-c is converted into a fluorescent derivative by reaction with 3-bromomethyl-6,7-dimethoxy-1-methyl-2(1H)-quinoxalinone. The derivative is separated on a reversed-phase column by isocratic elution of aqueous acetonitrile and monitored fluorimetrically. The ethyl ester is hydrolysed to E-64-c by carboxyl esterase and then derivatized in the same way as E-64-c. The limits of detection, at a signal-to-noise ratio of 3, of E-64-c and the ester are 500 pmol/ml in serum (10 microliters) and 300 pmol/g in muscle (20 mg), corresponding to ca. 0.5 pmol each in a 50-microliters injection volume. The method allows the determination of E-64-c and the ethyl ester in mouse serum and muscle after oral administration of these compounds.     

Rapid Spectrophotometric Method for Determining Erythrosine,Amaranth and Tartrazine in Ternary Mixtures

Abstract

A very simple spectrophotometric method using measurements at zero-crossing wavelength is described for resolving ternary mixtures of the food colorants Erythrosine (E-127), Amaranth (E-123) and Tartrazine (E-102). Calibration graphs are linear up to 14 mg/L of Erythrosine and 28 mg/L for Tartrazine and Amaranth. RSD of 0.80, 0.85 and 1.84% were obtained for nine standards of 8 mg/L of Erythrosine, 8 mg/L of Tartrazine and 8 mg/L of Amaranth, respectively. Detection limits of 0.052, 0.934 and 0.123 mg/L were obtained for Erythrosine, Tartrazine and Amaranth, respectively. This method was satisfactorily used for determining synthetic mixtures of these colorants in different ratios and it was successfully applied to a commercial product containing the three dyes; no separation step is required. The results were compared with those obtained by liquid chromatography and very similar values were found by both methods.     

Simultaneous spectrophotometric determination of Tartrazine, Sunset Yellow and Ponceau 4R in commercial products by partial least squares and principal component regression multivariate calibration methods

Three multivariate calibration methods, partial least squares (PLS-1 and PLS-2) and principal component regression (PCR), were proposed and successfully applied to the simultaneous determination of three dyes, Tartrazine (E-102), Sunset Yellow (E-110) and Ponceau 4R (E-124) in mixtures by ultraviolet-visible absorption spectrophotometry. The designed and optimized training set of calibration was applied to the determination of the three dyes in several synthetic mixtures, containing 1.6–20.0 mg/L of Tartrazine, 3.2–40.0 mg/L of Sunset Yellow and 3.2– 36.0 mg/L of Ponceau 4R. 94.5–105.3% recovery values were obtained. Three commercial foods that contained the three dyes were also satisfactorily analyzed without separation step. The results obtained by the application of the three chemometric approaches in the commercial products are discussed and compared with those obtained by an HPLC method and very similar values were found by all methods. Repeatability and reproducibility studies (with the Student’s and F tests) were achieved over two series of nine standards for each dye, showing no significant differences at the 95% confidence level. Received: 27 October 1997 / Revised: 9 January 1998 / Accepted: 24 January 1998     

Multicomponent analysis of chlorophenols by diode array derivative spectrophotometry

A multicomponent analysis method is proposed for the determination of chlorophenols by diode array derivative spectrophotometry. The method is based on formation of ion-pairs with tetrabutylammonium as counterion and extraction in chloroform at pH 9.1. Quantitative determinations (within the 2-20 mg/l. concentration range) of two-, three- and four-component mixtures were possible, using the first derivative spectra and a least-squares computer programme.     

用硝酸-亚硝酸钠双键异构化反应制备昆虫性信息素或其合成中间体

天然昆虫性信息素常是一定比例的两个或几个顺、反异构体的混合物。合成顺式烯烃已有许多有效的方法,如用Lindlar或P-2Ni催化剂氢化炔键,这些方法不仅产率高而且产物的纯度也高。本文报道应用HNO_3-NaN_2异构化双键的方法,使易得的顺式烯烃转化为顺、反异构体的混合物,并研究了温度对反应产物顺、反比例的影响。我们选用顺-3-辛烯醇-1(la)及其乙酸酯(lb),顺-9-十四烯醇-1-乙酸酯(2)和顺-11-十四烯醇-1-乙酸酯(3)进行实验。它们在各种温度下用HNO_3-NaNO_2转化可得不同比例的顺、反混合物(表1)。     

Solvent extraction of uranium(VI) by LIX-54 and its mixtures

Studies on solvent extraction of uranium(VI) by a commercially available chelating extractant LIX-54 (a -diketone derivative) (HA) and its mixtures with tri-n-butyl phosphate (TBP) in benzene diluent show quantitative extraction by a mixture of 5% LIX-54 and 5% TBP at pH 4.3. Influence of different proportions of LIX-54 or TBP in the mixtures on the extraction of the same metal ion has been studied. Pronounced synergism has been observed. The composition of the extracted species seems to be [UO₂(OH)(A)(HA)(TBP)] as determined from slope analysis. Slopes of the linear plots were computed employing regression analysis and variance in results has been shown.     

Simultaneous determination of germanium,arsenic, tin and antimony by molecular emission cavity analysis after hydride generation and gas chromatographic separation

Arsenic (0.1–5 μg), antimony (1–40 μg), tin (0.5–10 μg) and germanium (0.2–10 μg) are determined simultaneously by reduction to their hydrides with sodium tetrahydroborate(III), followed by gas chromatographic separation on a column of 10% E-301 silicone gum rubber on Porapak Q, and measurement of the emissions at 490 nm in an oxygen/hydrogen flame within a cavity. Detection limits for 1-ml samples are 35 ng As, 400 ng Sb, 85 ng Sn and 100 ng Ge. A more sensitive determination of arsenic (0.05–3 μg) and antimony (0.1–5 μg) in binary mixtures is also described; the detection limits are 15 ng As and 40 ng Sb.     

Simultaneous Determination of Acetaminophen with Orphenadrine Citrate,Ibuprofen or Chlorzoxazone in Combined Dosage Forms by Zero-Crossing Derivative Spectrophotometry

Abstract

A derivative spectrophotmetric procedure for the simultaneous determination of acetaminophen-orphenadrine citrate, acetaminophen-ibuprofen and acetaminophen-chlorzoxazone, binary mixtures is described. The procedure minimises the mutual interference between these drugs in mixtures and allows the determination of these compounds without a previous extraction step. The precision of the method, expressed as the relative standard deviation, is better than 4%. The method has been successfully applied to laboratory mixtures and commercial tablets containing these drugs.     

Photoinduced E to Z isomerization of tetraphenylethylene derivatives within organometallic supramolecular assemblies

Isolation of E-1,2-bis(4-bromophenyl)-1,2-diphenyl-ethylene from the E/Z isomer mixture obtained by a Mc Murry coupling reaction and reaction of this isomer with imidazole followed by N-alkylation with n Bu Br and anion exchange yielded the bisimidazolium tetraphenylethylene (TPE) derivative H_2-E-1(PF_6)_2.The reaction of H_2-E-1(PF_6)_2 with Ag_2O yielded the dinuclear metallarectangle[Ag_2(E-1)_2](PF_6)_2 where the two bis-NHC donors E-1 bridge two silver atoms.Irradiation of[Ag_2(E-1)_2](PF_6)_2 leads to E/Z isomerization of the di-NHC ligand and formation of Z-1 in the mononuclear complex[Ag(Z-1)]PF_6.Demetallation of the di-NHC ligand with NH_4Cl/NH_4PF_6 yielded bisimidazolium salt H_2-Z-1(PF_6)_2.The unique isomerization of the E-TPE derivative into its Z-isomer via metal complex formation/irradiation/demetallation cannot be achieved by irradiation of the individual imidazolium salt.The emissive properties of the TPE complexes[Ag_2(E-1)_2](PF_6)_2 and[Ag(Z-1)]PF_6 have been investigated.     

Enantioseparation of novel COX-2 anti-inflammatory drugs by capillary electrophoresis using single and dual cyclodextrin systems

A capillary electrophoresis method was developed for the enantioseparation of three novel cyclooxygenase-2 (COX-2) inhibitor drugs (E-6259, E-6036 and E-6087) with anti-inflammatory and analgesic activities using sulfobutyl ether-beta-cyclodextrin (SBE-beta-CD) as a chiral selector. The use of 50 mM sodium tetraborate at pH 9.2 with 30% v/v methanol, containing 7.1 mM SBE-beta-CD, as a background electrolyte (BGE) allowed the complete enantioseparation of the three neutral racemic mixtures (resolution = 2.4, 3.0 and 8.7, respectively) and their corresponding metabolites (oxidation products) in a single run. Migration times were shortened with some loss of enantioresolution by adding 1.75 mM dimethyl-beta-cyclodextrin (DM-beta-CD) to the previous BGE (dual CD system). The reversal of the migration order of E-6259 enantiomers in the dual CD system was also studied. Furthermore, the addition of DM-beta-CD to the BGE introduced a new chemoselectivity in the system that allowed E-6259 to be separated from the structurally similar compound E-6036.