High Pressure Liquid Chromatographic Determination of Monoand Disaccharides in Presweetened Cereals: Collaborative Study

1982 ◽  
Vol 65 (2) ◽  
pp. 256-264 ◽  
Author(s):  
Lucian C Zygmunt ◽  
◽  
E Anderson ◽  
B Behrens ◽  
R Bowers ◽  
...  

Abstract A collaborative study was conducted using a modified AOAC method (sugars in chocolate) for the determination of fructose, glucose, sucrose, and maltose in presweetened cereals by high pressure liquid chromatography (HPLC). Eight samples consisting of 6 products were analyzed in duplicate by the HPLC method and the AOAC Lane-Eynon method. The AOAC method was modified to use water-alcohol (1 + 1) and Sep-Pak C18 cartridges for sample cleanup. The HPLC results indicate precision comparable to the Lane-Eynon method and the chocolate method. The modified HPLC 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.


1980 ◽  
Vol 63 (3) ◽  
pp. 591-594
Author(s):  
Wesley R kreiser ◽  
Robert A Martin ◽  
◽  
R Bigornia ◽  
R Bond ◽  
...  

Abstract Four duplicate samples of cocoa-containing materials, a practice sample, and standards were submitted to the collaborators for theobromine and caffeine analysis by HPLC. In the method the samples are defatted with petroleum ether, and dried. The fat-free residue is then extracted with water and an aliquot is injected into the chromatograph. Compounds are quantitated by comparison with internal or external standards, either by peak height or peak area. Results for all the analyses showed that few of the values were more than 2 standard deviations from the mean. The method has been adopted as official first action.


1983 ◽  
Vol 66 (4) ◽  
pp. 864-866
Author(s):  
Eileen S Bargo ◽  
◽  
E Aranda ◽  
C Bonnin ◽  
S Hauser ◽  
...  

Abstract A reverse phase high pressure liquid chromatographic method for the determination of oxazepam in tablets and capsules was collaboratively studied by 9 laboratories. Collaborators were supplied with 6 samples that included synthetic and commercial formulations. Tablet and capsule composites are diluted with methanol and filtered. Oxazepam is determined at 254 nm by using a C18 column. Mean recoveries of oxazepam from synthetic tablet and capsule formulations were 97.2 and 99.0%, respectively. Mean coefficients of variation for tablets and capsules ranged from 1.85 to 2.86%. The method has been adopted official first action.


1982 ◽  
Vol 65 (1) ◽  
pp. 132-137
Author(s):  
Norlin W Tymes ◽  
◽  
G Briguglio ◽  
C Corcoran ◽  
R Everett ◽  
...  

Abstract Results of 11 laboratories are presented for the collaborative study of a proposed method for the quantitative reverse phase high pressure liquid chromatographic (HPLC) determination of physostigmine salicylate and physostigmine sulfate in pharmaceutical formulations. The samples consisted of commercial solution, injection, and ointment preparations, each containing one of the physostigmine salts. The physostigmine salt is extracted from ointments with acetonitrile after the ointment is dissolved in hexane. Liquid preparations are diluted directly. Physostigmine is determined at 254 nm on a C18 column by comparison with a physostigmine standard. Flurazepam hydrochloride is the internal standard. The method has been adopted official first action for the solution dosage form.


1977 ◽  
Vol 60 (4) ◽  
pp. 838-841 ◽  
Author(s):  
James E Thean ◽  
Walter C Funderburk

Abstract A normal phase high pressure liquid chromatographic (HPLC) method is presented for separating and determining sucrose in honeys. This method has been successfully applied to the analysis of field samples containing sucrose (0.63–8.44 wt %). Diluted honeys are filtered through a 0.45 μm membrane filter, and injected directly into the chromatograph. Samples are eluted from a μBondapak/carbohydrate column with acetonitrile-water (83+17) and quantitated with a refractive index detector. Average recovery of sucrose is 97%.


1983 ◽  
Vol 66 (5) ◽  
pp. 1063-1066
Author(s):  
Martin P Bueno ◽  
Melina C Villalobos

Abstract A reverse phase high pressure liquid chromatographic (HPLC) method for quantitating vitamin K1 in enzymatic hydrolysates of infant formula is described. The vitamin is extracted with n-pentane before determination by isocratic and isothermal reverse phase HPLC. Recovery of vitamin Ki added io 5 infant formulas ranged from 84 to 103%


1977 ◽  
Vol 60 (5) ◽  
pp. 1067-1069
Author(s):  
Manjeet Singh

Abstract A high pressure liquid chromatographic (HPLC) method has been developed for isolating and determining uncombined intermediates and subsidiary colors in Orange B. Samples of Orange B containing 0.1–0.3% naphthionic acid, 0.05–0.2 % phenylhydrazine-p-sulfonic acid, 0.2–0.8% pyrazolone-T and ethyl ester of pyrazolone-T, 0.2–1.0% 3-[(4-sulfo-l-naphthalenyl)-azo]-4-amino-l-naphthalenesulfonic acid, and 0.1–6.0% Orange K were prepared and analyzed by using this method. Recoveries ranged from 95 to 103%, except for the phenylhydrazine-p-sulfonic acid which ranged from 95 to 140%. Ten samples of Orange B were analyzed by conventional column and thin layer chromatographic methods as well as by the HPLC method. Good agreement was obtained for naphthionic acid, Orange K, and naphthionic acid plus the naphthionic acid subsidiary.


1979 ◽  
Vol 62 (5) ◽  
pp. 1004-1006
Author(s):  
Elmer H Hayes

Abstract A high pressure liquid chromatographic (HPLC) method for determining pentachlorophenol in formulations is described. Samples containing pentachlorophenol are accurately weighed in suitable volumetric flasks and diluted with dioxane. The sample is then injected onto a stainless steel column containing μBondapak C18. The mobile phase is 60% methanol/PIC A and 40% water/PIC A. This method is simple and eliminates many of the extractions required in other methods of analysis.


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).


1979 ◽  
Vol 62 (1) ◽  
pp. 176-185 ◽  
Author(s):  
David L Dunmire ◽  
Susan E Otto

Abstract A high pressure liquid chromatographic (HPLC) method has been developed which is fast, simple, specific, and reliable over a wide range of sugar concentrations in a variety of food matrices. With few exceptions, sample preparation is simple, requiring only a waterethanol extraction, followed by a rapid minicolumn cleanup before injection into the HPLC system. The majority of samples can be prepared for analysis within 1—1½ hr, and the following sugars are separated in <45 min: fructose, glucose, sucrose, maltose, lactose, melibiose, raffinose, and stachyose. This method is applicable to baby foods, cereals, chocolate products, chocolate sirups, cookies, health food products, molasses, preserves, processed fruits, and soy protein products.


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