Liquid Chromatographic Determination Of Polydextrose In Food Matrixes

1990 ◽  
Vol 73 (1) ◽  
pp. 51-53
Author(s):  
James B Noffsinger ◽  
Martha Emery ◽  
Daniel J Hoch ◽  
Jarmila Dokladalova

Abstract A liquid chromatographic (LC) method has been developed to determine the content of polydextrose, a water-soluble 1 calorie/g bulking agent, in food matrixes such as cookies, cakes, fruit spreads, and chocolate toppings. This analysis, which requires use of a blank matrix, provides a feasible means to control the manufacture of foods containing this additive and provides a component for the accurate determination of the caloric value of a particular food product. The method involves aqueous extraction of the polydextrose from the food matrix followed by separation on a carbohydrate analysis column. The LC system uses a mobile phase of 0.005M CaS04*2H2o and a refractive index detector for quantitation. Polydextrose recoveries from the food matrixes varied from 91.5 to 100.9% with assay precision, expressed as coefficient of variation, ranging from 0.7 to 4.3%. Each error estimate was derived from 5 parallel determinations. The present methodology is precise and selective in contrast to the modified classical phenol-sulfuric acid colorimetric method for assaying carbohydrates, which had been used for polydextrose determination in food matrixes in the past. Because the coefficient of variation frequently exceeded 10%, replicate analyses were necessary to achieve quantitation.

1984 ◽  
Vol 67 (5) ◽  
pp. 861-862 ◽  
Author(s):  
John Morawski ◽  
Glenn Kyle

Abstract A rapid, reliable separation and quantitation of zoalene (3,5-dinitroo-toluamide) from feeds is accomplished by using reverse phase liquid chromatography (LC) and ultraviolet detection. An extraction technique which is similar to the present AOAC official colorimetric method is used before chromatographic analysis. This extraction is followed by an activated alumina cleanup and LC to separate zoalene from feed matrix. The methodology was applied to a variety of spiked feed matrices, and yielded good recoveries. Liquid chromatographic results were shown to correlate with colorimetric determinations.


1984 ◽  
Vol 67 (3) ◽  
pp. 492-493
Author(s):  
Stephen C Slahck ◽  
◽  
A A Carlstrom ◽  
L T Chenery ◽  
N D Ellis ◽  
...  

Abstract An LC method for the determination of methiocarb in methiocarb technical and formulated products has been subjected to a collaborative study with 9 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with acetophenone as an internal standard. Collaborators were furnished samples of technical, 75% wettable powder, 75% seed treater, 75% concentrate, and 50% hopper box treater. Coefficient of variation values obtained on the 5 samples were 0.71, 0.83, 0.62, 1.57, and 0.82%, respectively. The method has been adopted official first action.


1983 ◽  
Vol 66 (2) ◽  
pp. 284-286
Author(s):  
Thomas D Macy ◽  
Andrew Loh

Abstract A high pressure liquid chromatographic (HPLC) method has been developed to determine monensin in feed premixes. The method is simple and rapid. Monensin is extracted with methanol-water and determined in the extracting solution by HPLC. Average recovery for monensin from a 13.2% premix sample was 103% (coefficient of variation (CV), 2.6%) by HPLC and compares with the value of 100% (CV, 3.4%) obtained by the turbidimetric bioassay method.


1972 ◽  
Vol 55 (6) ◽  
pp. 1219-1222
Author(s):  
Victor W Winkler ◽  
John M Yoder

Abstract A method for the quantitative determination of menadione bisulfite addition products in feed premixes is presented. The menadione bisulfite compound is extracted with methanol from the premix and is determined by gas chromatography directly without pretreatment with alkali. The principle of the method is on-column pyrolysis of menadione bisulfite and subsequent gas chromatographic analysis of the pyrolytic product, menadione.


1988 ◽  
Vol 71 (5) ◽  
pp. 1054-1056 ◽  
Author(s):  
Joel E Houglum ◽  
Richard D Larson ◽  
Rose M Neal

Abstract A reverse-phase liquid chromatographic method for the assay of sulfamethazine (SMZ) in feeds is described. Feed samples are extracted with 50% methanol solution, centrifuged, filtered, and diluted when necessary, and chromatographed on a C-18 column. Samples are eluted with a mobile phase of 20% methanol and 80% of a solution containing acetic acid and tetramethylammonium chloride. The average recovery from spiked samples was 97.2% with a coefficient of variation of 1.2%. Linearity was very good (correlation coefficient 0.9997). Within-day and between-day coefficients of variation averaged 1.3 and 2.6%, respectively. The results for samples assayed by this method compared closely with the results from the same extracts assayed by the AOAC colorimetric method


1988 ◽  
Vol 71 (3) ◽  
pp. 480-484 ◽  
Author(s):  
Michel R Lapointe ◽  
Huguette Cohen

Abstract A high-speed liquid chromatographic (LC) method using post-column derivatization is described for the determination of monensin, narasin, and salinomycin in a variety of animal feeds. The ionophores are extracted with hexane-ethyl acetate (90 + 10). A portion of the sample is evaporated, diluted to a known volume, and analyzed using a 6 cm 3 μm C18 column and an absorbance detector after post-column reaction with vanillin. The method has been applied to poultry and swine feeds with levels of 3-100 ppm added antibiotic. A comparison was also carried out with medicated poultry feed and beef feed lot supplement samples previously analyzed by 2 separate bioassay methods for monensin and salinomycin, respectively. Recoveries for the LC method ranged from 92.1 to 103% with an average recovery of 98.1% and a coefficient of variation of 3.65%.


1984 ◽  
Vol 67 (4) ◽  
pp. 768-770
Author(s):  
Allan D Davidson ◽  
◽  
C Barry ◽  
J Carmany ◽  
A F Grigor ◽  
...  

Abstract A second collaborative study with 6 collaborators was conducted on the AOAC official first action method for measuring nitrogen derived from urea, methylenediurea (MDU), and dimethylenetriurea (DMTU). No variations were made. The collaborators made single determinations on 2 separate days on 5 sets of paired samples. The mean coefficients of variation for the completed study were 4.22% for urea, 5.08% for MDU, and 5.48% for DMTU, which are only slightly higher than the values reported in the first study: urea, 3.24%; MDU, 3.48%; and DMTU, 6.56%. The method has been adopted official final action.


1970 ◽  
Vol 16 (7) ◽  
pp. 587-593 ◽  
Author(s):  
H E Sine ◽  
M J McKenna ◽  
T A Rejent ◽  
M H Murray

Abstract A method is presented for the rapid gas chromatographic determination of barbiturates and glutethimide in serum, suitable for use in clinical emergencies. The sample is prepared for gas chromatography by acidification and a single extraction with chloroform. From 70 to 100% of the various barbiturates and glutethimide are analytically recovered, with a coefficient of variation of 8 to 10% for the method. During a 10-month clinical evaluation (87 requested determinations), 34 analyses (39% of the samples submitted) were positive for barbiturates, glutethimide, or both.


1978 ◽  
Vol 61 (5) ◽  
pp. 1070-1073
Author(s):  
Robert B Hagel

Abstract A high pressure liquid chromatographic (HPLC) method has been developed to determine lasalocid in premixes. The method is simple and rapid, requiring an extraction of the drug and separation of insoluble material before HPLC. Elution times are typically <10 min per sample. The average recoveries for lasalocid at the 16.5 and 50% levels were 100.2±2 and 100.0±2%, respectively. The precision of the method (coefficient of variation = 0.02) compares favorably with that of the approved bioassay (coefficient of variation = 0.06).


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