Determination of Polydextrose (Polymer) and Residual Monomers in Polydextrose by Liquid Chromatography

1991 ◽  
Vol 74 (3) ◽  
pp. 571-574
Author(s):  
John W Thomas ◽  
Donna L Brown ◽  
Daniel J Hoch ◽  
John J Leary ◽  
Jarmila Dokladalova

Abstract A simple, liquid chromatographic method has been developed for determination of the reduced-calorie food additive polydextrose—a water soluble, 1 kilocalorie/gram bulking agent used extensively for manufacture of low-calorie food products. The method allows rapid determination of polydextrose content as well as determination of the minor components: dextrose, sorbitol, and 2 isomeric anhydroglucoses in bulk samples of polydextrose. The proposed method is superior to current Food Chemical Codex (FCC) methodologies for determination of polydextrose (phenol sulfuric acid spectrophotometry) and for determination of residual monomers [gas chromatographic (GC) determination as their trimethylsilyl derivatives]. The proposed method is more precise, considerably faster, and is safer to execute. The method uses a resin-based cation exchange column, 0.001N sulfuric acid mobile phase, and differential refractive index detection. Analyte response curves were linear; and data displayed good precision with coefficients of variation ranging from 1.1 to 1.6%. The efficiency, specificity, precision, and ruggedness of the method make it amenable to implementation in a routine quality control operation.

2016 ◽  
Vol 13 (2) ◽  
pp. 447-457 ◽  
Author(s):  
Baghdad Science Journal

High-performance liquid chromatographic methods are used for the determination of water-soluble vitamins with UV-Vis. Detector. A reversed-phase high-performance liquid chromatographic has been developed for determination of water-soluble vitamins. Identification of compounds was achieved by comparing their retention times and UV spectra with those of standards solution. Separation was performed on a C18 column, using an isocratic 30% (v/v) acetonitril in dionozed water as mobile phase at pH 3.5 and flow rate 1.0m/min. The method provides low detection and quantification limits, good linearity in a large concentration interval and good precision. The detection limits ranged from 0.01 to 0.025µg/ml. The accuracy of the method was tested by measuring average recovery values ranged between 94% - 101 %. For standerd solution, and 93%-99% of honey bee samples.


2007 ◽  
Vol 90 (2) ◽  
pp. 384-390 ◽  
Author(s):  
Samy Emara ◽  
Alaa El-Gindy ◽  
Mostafa K Mesbah ◽  
Ghada M Hadad

Abstract A very simple liquid chromatographic technique was developed and validated for the simultaneous determination of 2 antihistaminic drugs, loratadine (LT) and terfenadine (TR), and their major active metabolites, desloratadine (DL) and fexofenadine (FX), respectively, in human serum. LT, DL, TR, and FX from directly injected serum samples were enriched on a protein-coated RP8 silica precolumn (10 4.6 mm id) while serum constituents, such as proteins and salts, were eluted to waste. Using an online column-switching system, the drugs and their metabolites were quantitatively transferred and separated on a second analytical column (Shim-pack 5 μm particle size cyanopropyl, 250 × 4.6 mm id) followed by ultraviolet detection at 243 nm for LT and DL and 220 nm for TR and FX. Very good precision, accuracy, and linearity were obtained over the range of 101000 ng/mL for LT and DL, 10500 ng/mL for TR, and 103000 ng/mL for FX in human serum. High extraction recoveries from serum ranging from 96.03 to 98.19, 95.44 to 97.26, 95.61 to 98.17, and 95.60 to 97.89 for LT, DL, TR, and FX, respectively, were obtained.


Author(s):  
Minwei Zhang† ◽  
Hong Ping† ◽  
Xianyi Cao ◽  
Hongkun Li ◽  
Fengrui Guan ◽  
...  

1984 ◽  
Vol 30 (5) ◽  
pp. 784-787 ◽  
Author(s):  
R A Gibson ◽  
L Lattanzio ◽  
H McGee

Abstract Metronidazole and its known metabolites in plasma can be rapidly separated by a "high-pressure" liquid-chromatographic method that can also be adapted for rapid determination of tinidazole. Samples deproteinized with trichloroacetic acid (50 g/L final concentration) undergo isocratic separation on a reversed-phase C18 column eluted with an 8/92 (by vol) mixture of acetonitrile/KH2PO4 (5 mmol/L, pH 3.0). The method is sensitive, reliably detecting as little as 25 micrograms of metronidazole and (or) its metabolites per milliliter of plasma. The detector response varied linearly with concentration for all compounds tested over a wide range (25-500 micrograms/L). Within-day and between-day variation was generally less than 2.5% for all concentrations of all compounds tested. Various other antibiotics tested did not interfere.


1997 ◽  
Vol 80 (1) ◽  
pp. 25-30 ◽  
Author(s):  
Catharina Y W Ang ◽  
Luo Wenhong

Abstract A rapid and sensitive liquid chromatographic (LC) method was developed for the determination of am- picillin residues in raw bovine milk, processed skim milk, and pasteurized, homogenized whole milk with vitamin D. Milk samples were deprote- inized with trichloroacetic acid (TCA) and acetonitrile. After centrifugation, the clear supernatant was reacted with formaldehyde and TCA under heat. The major fluorescent derivative of ampicillin was then determined by reversed-phase LC with fluorescence detection. Average recoveries of ampicillin fortified at 5,10, and 20 ppb (ng/mL) were all >85% with coefficients of variation <10%. Limits of detection ranged from 0.31 to 0.51 ppb and limits of quantitation, from 0.66 to 1.2 ppb. After appropriate validation, this method should be suitable for rapid analysis of milk for ampicillin residues at the tolerance level of 10 ppb.


1967 ◽  
Vol 50 (2) ◽  
pp. 334-338
Author(s):  
Duane H Strunk ◽  
A A Andreasen

Abstract Results are given on a collaborative study in which a zinc dibenzyldithiocarbamate (ZDBT) colorimetric method is used to measure copper in alcoholic products such as high wine, spirits, gin, whisky, brandy, rum, and wine. In this method, the sample is made ca 0.SN with sulfuric acid, and carbon tetrachloride containing 0.2% ZDBT is added. The colored copper-ZDBT complex is extracted in the carbon tetrachloride and measured at 438 mμ against a similar carbon tetrachloride extract of a blank. Data show good precision, and it is recommended that the ZDBT method be adopted as official, first action.


1972 ◽  
Vol 55 (1) ◽  
pp. 146-148
Author(s):  
Clyde E Wells

Abstract Eight laboratories collaboratively studied a method for the quantitative GLC determination of d- and l-amphetamine in tablets. The drugs are separated from tablet excipients by column chromatography and reacted with Ntrifluoroacetyl-( 0-prolyl chloride, and the resulting derivatives are analyzed by GLC. The samples consisted of commercial d-amphetamine sulfate tablets (with and without butabarbital), dl-amphetamine sulfate tablets, and a mixed d- and l-amphetamine sulfate standard. Recoveries were acceptable, and the standard deviations never exceeded 0.64%. The results demonstrate that the method gives good precision and accuracy, and the method is recommended for adoption as official first action.


1973 ◽  
Vol 56 (5) ◽  
pp. 1277-1280
Author(s):  
Victor W Winkler

Abstract A GLC method for the determination of menadione bisulfite addition products in feed premixes was tested by 8 laboratories. Menadione sodium bisulfite complex (trihydrate) is extracted with methanol containing 1 mg diethyl phthalate/ml as internal standard and injected directly onto a 2% OV-17 (silylated) GLC column. The principle of the method is on-column pyrolysis of menadione bisulfite and subsequent GLC analysis of the pyrolytic product, menadione. The method is simple, rapid, and free from interference. The average recovery values for 4 samples at 16.0, 14.4, 4.0, and 3.6 g/lb ranged from 95.8 to 100.4% with coefficients of variations between 5.5 and 6.5%. The method has been adopted as interim official first action.


1980 ◽  
Vol 63 (3) ◽  
pp. 460-461
Author(s):  
Saidul Z Qureshi ◽  
Fadhil M Najib ◽  
Fahmi A Mohammed

Abstract An ion exchange method to determine the alkalinity of water-soluble tea ash containing high levels of manganese is described. A chromatographic column containing a strong cation exchange resin (20–50 mesh) in Na+ form, with a bed volume of 5 mL is used. The present ion exchange method is compared to pH titrations and also to the official AOAC methods (31.012, 31.015, 31.016). Results with the new method are accurate and precise.


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