High Performance Liquid Chromatographic Determination of Intermediates and Two Reaction By-Products in FD&C Red No. 40: Collaborative Study

1981 ◽  
Vol 64 (2) ◽  
pp. 324-331
Author(s):  
Elizabeth A Cox ◽  
George F Reed ◽  
◽  
L Bille ◽  
R Bischof ◽  
...  
Keyword(s):  
High Performance ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Repeatability And Reproducibility ◽  
Liquid Chromatographic ◽  
By Products

Abstract Nine laboratories participated in a collaborative study of an ion exchange high performance liquid chromatographic procedure for determining the intermediates and 2 reaction by-products in FD&C Red No. 40: cresidine sulfonic acid (CSA), Schaeffer’s Salt (SS), 4,4’-(diazoamino)bis(5-methoxy-2-methylbenzenesulfonic acid) (DMMA), and 6,6’-oxybis(2- naphthalenesulfonic acid) (DONS), respectively. The repeatability and reproducibility standard deviations (absolute) found in the study were 0.012 and 0.019 for CSA at the 0.2% level, 0.004 and 0.006 for DMMA at the 0.1% level, 0.067 and 0.087 for DONS at the 1% level, and 0.015 and 0.020 for SS at the 0.3% level, respectively. The method has been adopted official first action.

High Performance Liquid Chromatographic Determination of Intermediates and Reaction By-Products in FD&C Yellow No. 5: Collaborative Study

1982 ◽  
Vol 65 (4) ◽  
pp. 933-940
Author(s):  
Elizabeth A Cox ◽  
Foster D Mcclure ◽  
◽  
S Bell ◽  
R Beswick ◽  
...  
Keyword(s):  
High Performance ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Sulfanilic Acid ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Repeatability And Reproducibility ◽  
Liquid Chromatographic ◽  
By Products

Abstract Eight laboratories participated in a collaborative study of an ion exchange high performance liquid chromatographic procedure for determining the intermediates and 2 reaction by-products in FD&C Yellow No. 5: phenylhydrazine-p-sulfonic acid (PHSA), sulfanilic acid (SA), l-(4-sulfophenyl)-3- carboxy-5-hydroxypyrazolone (PyT), l-(4-sulfophenyl) - 3 -ethylcarboxy-5-hydroxypyrazolone (EEpyT), and 4,4'-(diazoamino)-dibenzenesulfonic acid (DAADBSA). The repeatability and reproducibility standard deviations (absolute) found in the study were 0.0134 and 0.0263 for PHSA at the 0.1% level, 0.0246 and 0.0256 for SA at the 0.2% level, 0.0124 and 0.0149 for EEpyT at the 0.1% level, 0.0212 and 0.0258 for PyT at the 0.2% level, and 0.0234 and 0.0373 for DAADBSA at the 0.2% level. The method was adopted official first action.

High Performance Liquid Chromatographic Determination of Sulfanilic Add, Schaeffer’s Salt, 4,4´-(Diazoamino)-DibenzenensuIfonic Acid, and 6,6´-Oxybis(2-Naphthalenesulfonic Acid) in FD&C Yellow No. 6: Collaborative Study

1980 ◽  
Vol 63 (1) ◽  
pp. 61-68
Author(s):  
Elizabeth A Cox ◽  
◽  
R Beswick ◽  
L Bille ◽  
G Gasper ◽  
...  
Keyword(s):  
High Performance ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Sulfanilic Acid ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract Eight laboratories participated in a collaborative study of a high performance liquid chromatographic procedure for determining sulfanilic acid, Schaeffer's salt, 4,4´-(diazoamino)-dibenzenesulfonic acid (DAADBSA), and 6,6´-oxybis(2-naphthalenesulfonic acid) (DONS) in FD&C Yellow No. 6. The standard deviations for one analysis in any one laboratory for sulfanilic acid at 0.2%, Schaeffer's salt at 0.26%, DAADBSA at 0.1%, and DONS at 1.0% were 0.015%, 0.014%, 0.018%, and 0.077%, respectively. The method has been adopted as official first action.

Reverse Phase High Performance Liquid Chromatographic Determination of Phenprocoumon in Tablets

1982 ◽  
Vol 65 (3) ◽  
pp. 753-756
Author(s):  
Walter F Schmidt
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase ◽  
Assay Procedure ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic procedure has been developed for the assay of phenprocoumon in tablets. In comparison to the present official USP assay procedure, it is equivalent in precision and accuracy and is faster and more specific. A mobile phase consisting of a 1% solution of acetic acid in acetonitrile-water (4 + 3) separates phenprocoumon from warfarin internal standard on a 6 μm octadecylsilane (ODS) column with UV detection at 311 nm. The method enables the concurrent determination of phenprocoumon and possible contaminants such as salicylic acid.

High Performance Liquid Chromatographic Determination of Carbohydrates in Chocolate: Collaborative Study

1980 ◽  
Vol 63 (3) ◽  
pp. 595-599
Author(s):  
W Jeffrey Hurst ◽  
Robert A Martin ◽  
◽  
M Bueno ◽  
H Clemente ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Adequate Method

Abstract A collaborative study determining sucrose, glucose, fructose, maltose, and lactose in chocolate products was conducted using a previously published high performance liquid chromatographic (HPLC) method. Five samples (2 milk chocolates, 1 dark chocolate, 1 powdered mix, and 1 sirup) were analyzed in duplicate by 7 collaborators. The results indicate adequate method precision. In addition, the HPLC method allows for the simultaneous determination of 5 saccharides in chocolate products in 15 min. The method has been adopted as official first action.

Liquid-chromatographic determination of aminoglutethimide in plasma.

1983 ◽  
Vol 29 (6) ◽  
pp. 1104-1105 ◽  
Author(s):  
B A Robinson ◽  
F N Cornell
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Ammonium Phosphate ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple, rapid "high-performance" liquid-chromatographic procedure is presented for the determination of aminoglutethimide in plasma. After precipitation of the protein with acetonitrile, an aliquot of the supernate is injected directly onto a radially compressed, reversed-phase column. The aminoglutethimide is isocratically eluted with a mobile phase of acetonitrile/water/tert-butyl ammonium phosphate. The method is both accurate and precise and has been in routine use in our laboratory for more than 12 months.

Simultaneous liquid-chromatographic determination of vitamin K1 and vitamin E in serum.

1989 ◽  
Vol 35 (12) ◽  
pp. 2285-2289 ◽  
Author(s):  
B E Cham ◽  
H P Roeser ◽  
T W Kamst
Keyword(s):  
Vitamin E ◽  
Human Serum ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Tocopheryl Acetate ◽  
Vitamin K1 ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We describe a high-performance liquid chromatographic procedure for the simultaneous measurement of vitamins K1 and E in human serum. Delipidated human serum (free of vitamins K1 and E) was used to make standard solutions of these vitamins, and cetyl naphthoate and alpha-tocopheryl acetate were the internal standards for vitamin K1 and vitamin E, respectively. A simple, novel separation method utilizing liquid-liquid partition chromatography was used as a preparative "clean-up" procedure. Cetyl naphthoate and vitamin K1 (after post-column reduction) were detected by fluorescence, alpha-tocopheryl acetate and vitamin E by ultraviolet absorption. Sensitivity (detection limit) of the assay was 30 pg for vitamin K1 and 5 ng for vitamin E per injection. The method is specific, precise, and more rapid than previously described procedures. Within- and between-assay CVs were 8.1% and 12.9%, respectively, for vitamin K1; 3.5% and 6.0%, respectively, for vitamin E. Analytical recoveries of vitamins K1 and E were 80% and 93%, respectively, from serum and from delipidated serum (standards). The average neonatal serum concentration of vitamin K1 was 83 ng/L, 2.5 mg/L for vitamin E; for normolipidemic adults, the values were 343 ng/L and 7.9 mg/L, respectively, and for hyperlipidemic adults, 541 ng/L and 11.1 mg/L, respectively.

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