Determination of Aflatoxins in Peanut Butter, Using Two Liquid Chromatographic Methods: Collaborative Study

1984 ◽  
Vol 67 (2) ◽  
pp. 312-316
Author(s):  
Alfred D Campbell ◽  
Octave J Francis ◽  
Roberta A Beebe ◽  
Leonard Stoloff ◽  
◽  
...  

Abstract Two methods for determining aflatoxins in peanut butter, one using normal phase and the other reverse phase liquid chromatography (LC), were studied by 8 and 10 collaborators, respectively. Fluorescence detection was used for the determinative step in both methods. For reverse phase LC, aflatoxins B1 and G1 were converted to B2a and G2a; for normal phase LC, a silica gel-packed flow cell was placed in the irradiating light path of the detector. The samples included spiked and naturally contaminated peanut butter with total aflatoxin levels from about 5 to 20 ng/g and controls in a balanced pair design. For the normal phase LC method, recoveries of B1, B2, G1, and G2 from spiked samples averaged 79, 92, 74, and 88%, respectively; for the reverse phase method, the recoveries were 103, 104, 89, and 163%. For the normal phase LC method, pooled repeatabilities were 20, 23, 28, and 17% for B1, B2, G1, and G2, respectively; for the reverse phase method, the repeatabilities were 19, 22, 38, and 31%. For the normal phase method, pooled reproducibilities were 34, 33, 39, and 34% for B1, B2, G1, and G2, respectively; for the reverse phase method, the reproducibilities were 32, 46, 51, and 52%. Both methods show an improved limit of detection and better within-laboratory precision over current AOAC methods; however, between-laboratory precision is no better, and the reverse phase method shows evidence of interferences being measured. For these reasons and because of no benefits of present value, neither method was submitted for adoption as official first action.

1984 ◽  
Vol 67 (6) ◽  
pp. 1118-1120
Author(s):  
Ting Susan ◽  
◽  
R L Brown ◽  
L A Dougherty ◽  
J B Schepman ◽  
...  

Abstract A reverse phase liquid chromatographic method for the determination of methyldopa, methyldopa-hydrochlorothiazide, and methyldopachlorothiazide in tablets was collaboratively studied by 8 laboratories. Each collaborator received 20 samples that included drug substance, synthetic and commercial tablet compositions. The overall repeatability and reproducibility standard deviations for commercial tablets were 1.11 and 1.75% for methyldopa, 0.96 and 1.62% for chlorothiazide, and 1.21 and 2.15% for hydrochlorothiazide, respectively. The overall recoveries of methyldopa, chlorothiazide, and hydrochlorothiazide added to synthetic tablets were 100.78, 100.70, and 101.34%, respectively. The method has been adopted official first action.


1984 ◽  
Vol 67 (2) ◽  
pp. 218-221 ◽  
Author(s):  
Milda J Walters ◽  
◽  
N Falcone ◽  
K G Hanel ◽  
E H Jefferson ◽  
...  

Abstract A normal phase liquid chromatographic (LC) method for determining the hydrocortisone content of bulk drug substance, tablet composites, and individual tablets was subjected to a collaborative study by 6 laboratories. The results showed a mean recovery of 98.5% for an authentic tablet formulation and reproducibility coefficients of variation of 0.97, 1.6, and 2.7% for bulk drug substance, tablet composites, and individual tablets, respectively. Infrared (IR) and thin layer chromatographic (TLC) identification tests, also included in the collaborative study, were satisfactory. The LC method for determining hydrocortisone in bulk drug substance, tablet composites, and individual tablets, with IR and TLC identification, has been adopted official first action.


1988 ◽  
Vol 71 (5) ◽  
pp. 1068-1071 ◽  
Author(s):  
Frans J. E. M Kuppers ◽  
Jan A Jans

Abstract The sorbate and benzoate contents of commercial fresh cheese (quarg) samples are determined by reverse-phase liquid chromatography following extraction with a methanol-acetate buffer pH 4.5 mixture (37 + 63). The mobile phase is acetonitrile-acetate buffer pH 4.5 (20 + 80), the effluent flow rate is maintained at 1.0 mL/min, and the detector is set at 232 nm. Recoveries from quarg spiked at the 5-50 mg/kg level ranged from 95 to 99%, which compares favorably with methods previously published. Precision averaged 2-5% RSD, whereas the limit of detection was 0.3 mg/kg (sorbic acid) and 1.0 mg/kg (benzoic acid).


1984 ◽  
Vol 67 (5) ◽  
pp. 924-926
Author(s):  
John L Van Ackeren ◽  
Richard M Venable ◽  
Irving W Wainer

Abstract A method for separating and determining pilocarpine and 2 degradation products was developed and subjected to collaborative study. Pilocarpine, isopilocarpine, and pilocarpic acid were isolated on a reverse phase liquid chromatographic phenyl bonded column and detected by UV spectrophotometry at 220 nm. Nine collaborators received commercial samples labeled to contain 2,1, and 0.5% pilocarpine and a 2% practice sample. The collaborative results for pilocarpine were excellent; coefficients of variation ranged from 3.20 to 4.10%. The method was adopted official first action for determination of the active component, pilocarpine, in the presence of isopilocarpine and pilocarpic acid. Although quantitative results for the degradation products were not as good, the method is suitable as a limits test for these substances.


1989 ◽  
Vol 72 (4) ◽  
pp. 562-563
Author(s):  
Edward J Wojtowicz

Abstract Seven laboratories participated in a collaborative study to analyze, in duplicate, 2 synthetic formulations and 2 commercial preparations, labeled to contain 3% clioquinol. Clioquinol is determined as its nickel (II) complex by reverse-phase liquid chromatography on a phenylbonded column with a mobile phase of acetonitrile-methanol-water, containing ammonium acetate and nickel chloride. Detection is at 273 nm and diphenylamine is added as an internal standard. Mean recoveries were 99.1 and 101.1%, respectively, for the ointment and cream synthetic preparations and 96.7 and 99.7%, respectively, for the commercial ointment and cream. All results are consistent with the variability of other methods at this concentration range. The method has been approved interim official first action


1987 ◽  
Vol 70 (2) ◽  
pp. 212-214
Author(s):  
David J Krieger

Abstract A reverse phase liquid chromatographic method previously reported for the determination of acetaminophen in tablets was collaboratively studied by 5 laboratories. Each collaborator received duplicate samples of a synthetic tablet formulation and 3 powdered commercial tablet composites. The composites represented single-component and multi-component proprietary products and a single-component generic product. The pooled repeatability (CVD„) and reproducibility (CVDJ values for the proprietary tablets were 0.89 and 1.34%, respectively. For the generic tablets, these values were 0.66 and 0.74%, respectively. The pooled recovery value for acetaminophen added to the synthetic formulation was 98.9 ± 0.7% (n = 10) with a CV of 0.75%, CVD„ of 0.37%, and CVD„ of 0.78%. The overall repeatability of the method was 0.64%, and the overall reproducibility was 0.95%. The method has been adopted official first action.


1988 ◽  
Vol 71 (5) ◽  
pp. 957-961 ◽  
Author(s):  
Walter E Paulsch ◽  
Eric A Sizoo ◽  
Hans P Van Egmond

Abstract A liquid chromatographic (LC) method was developed for the determination of aflatoxins in feedstuffs containing citrus pulp. The feedstuff sample is extracted with chloroform, followed by Sep-Pak Florisil cartridge cleanup and Sep-Pak C18 cartridge cleanup. The final eluate (water-acetone, 85 + 15, v/v) is submitted to reverse-phase liquid chromatography with water-methanol-acetonitrile (130 + 70 + 40, v/v/v) as mobile phase and postcolumn derivatization with iodine. Citrus components are removed from the extract efficiently. The limit of detection for aflatoxin B1 is< 1 μg/kg. Other aflatoxins can also be detected and measured. Recoveries of aflatoxins B1 B2, G,1 and G2 for dairy rations spiked at 13, 5, 10, and 4 μg/kg were 87, 86, 81, and 82%, respectively. Corresponding coefficients of variation were 3.1, 3.6, 5.2, and 3.8%, respectively.


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.


1988 ◽  
Vol 71 (1) ◽  
pp. 53-55 ◽  
Author(s):  
Kenneth M Weaver ◽  
Michael E Neale ◽  
Ann Laneville

Abstract A method was developed for the detection and quantitation of piperine in Piper nigrum. A reverse-phase liquid chromatographic system equipped with a C18 column with detection at 340 nm was used. A rapid 1 h acetone extraction followed by solvent dilution was used to avoid sample cleanup. The detection limit is 3 ng injected piperine, with 97.5-100.5% recovery of added piperine.


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