Assay of Formulations Containing 2,4-D and/or Picloram by Direct Injection High Pressure Liquid Chromatography

1979 ◽  
Vol 62 (2) ◽  
pp. 297-303
Author(s):  
Timothy S Stevens
Keyword(s):  
High Pressure ◽  
Chromatographic Method ◽  
Direct Injection ◽  
Hplc Method ◽  
Dichlorophenoxyacetic Acid ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
2,4 Dichlorophenoxyacetic Acid ◽  
Liquid Chromatographic

Abstract A rapid and precise fully automated, direct injection high pressure liquid chromatographic method is described for assaying liquid formulations of 2,4-dichlorophenoxyacetic acid (2,4-D) and/or picloram (4-amino-3,5,6-trichloropicolinic acid). The method is specific for the 2,4-D and picloram isomers. No sample preparation is needed, triplicate assays can be performed in 1 hr, and precision is about 1% relative at the 95% confidence level. Compounds are separated on a 9 mm id reverse phase microparticulate column with an eluant of ace* tonitrile-water (1+4) , buffered at pH 2.95. No bias was observed between this method and the official final action HPLC method for picloram and 2,4-D in picloram-2,4-D mixtures, 6.B09-6.B12.

High Pressure Liquid Chromatographic Determination of Furazolidone in Turkey Tissue

1979 ◽  
Vol 62 (2) ◽  
pp. 257-261
Author(s):  
Betty-Ann Hoener ◽  
Gloria Lee ◽  
William Lundergan
Keyword(s):  
High Pressure ◽  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic method for determining furazolidone in turkey tissue has been developed. Tissues are ground with methanol and centrifuged. For lower levels of furazolidone, 2—40 ppb, the supernate is evaporated to dryness and redissolved before it is injected onto the liquid chromatographic column. Using a reverse phase column and an ultraviolet absorption detector set at 365 nm, the assay is linear over the concentration range 2—400 ppb with a coefficient of variation of <4%. Average recovery from fortified tissues was 96% with a coefficient of variation of 6% at the 50-400 ppb level, and 105% with a coefficient of variation of 11% at the 2—40 ppb level.

Isomer Specific Assay of Ester and Salt Formulations of 2,4-Dichlorophenoxyacetic Acid by High Pressure Liquid Chromatography: Collaborative Study

1978 ◽  
Vol 61 (5) ◽  
pp. 1163-1165 ◽  
Author(s):  
Timothy S Stevens ◽  
Norman E Skelly ◽  
Robert B Grorud
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Internal Standard ◽  
Dichlorophenoxyacetic Acid ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Standard Solution ◽  
2,4 Dichlorophenoxyacetic Acid ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) assay of ester and salt formulations of 2,4-D has been collaboratively studied. The method is specific for 2,4-D isomer and resolves all known impurities from 2,4-D and the internal standard p-bromophenol. In situ saponification, at room temperature, is performed by adding a combined saponification-internal standard solution to ester products. The same saponification- internal standard solution is added to amine salts and the analytical standard. The injected aqueous potassium salt solution of 2,4-D is then converted to the acid form by an acidic buffered mobile solvent of 20% acetonitrile in water. Optimum chromatography is attained by a mobile solvent pH of 2.95 in a reverse phase microparticulate column, by ion suppression. Each of the 9 collaborators received 3 different ester and 2 different amine formulations of 2,4-D. The coefficients of variation of 2,4-D acid equivalent ranged from 1.22 to 1.59%. The method has been adopted as official first action.

Preparation and Spectral Analysis of 3,3',4,4'-Tetrachloroazobenzene and the Corresponding Azoxy and Hydrazo Analogs

1979 ◽  
Vol 62 (4) ◽  
pp. 746-750
Author(s):  
M T Stephen Hsia ◽  
Charles F Burant
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Chromatographic Method ◽  
Lithium Aluminum Hydride ◽  
Aluminum Hydride ◽  
Lithium Aluminum ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Hydride Reduction ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract An efficient preparation was developed for 3,3',4,4'-tetrachloroazobenzene and the corresponding azoxy and hydrazo derivatives, based on the lithium aluminum hydride reduction of 3,4-dichIoronitrobenzene. Batches were analyzed for purity by using a reverse phase high pressure liquid chromatographic method. All 3 compounds can be synthesized in gram quantities with 97–99% purity. Detailed mass, infrared, and nuclear magnetic resonance spectral analyses are presented.

Determination of Uncombined Intermediates in FD&C Yellow No. 6 by High-Pressure Liquid Chromatography

1974 ◽  
Vol 57 (2) ◽  
pp. 358-359
Author(s):  
Manjeet Singh
Keyword(s):  
High Pressure ◽  
Chromatographic Method ◽  
Sulfanilic Acid ◽  
Sunset Yellow ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Two Samples ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A high-pressure liquid chromatographic method is presented for the isolation and determination of uncombined intermediates in FD&C Yellow No. 6 (sunset yellow FCF, CI. No. 15895). Samples of FD&C Yellow No. 6 containing 0.1-0.4% sulfanilic acid, 0.1-0.4% 6-hydroxy-2-naphthalenesulfonic acid, and 0.3— 1.0% 6,6'-oxybis(2-naphthalenesulfonic acid) were prepared and analyzed using this method. Recoveries ranged between 94 and 101%. Twenty-two samples of FD&C Yellow No. 6 were analyzed by the conventional column elution chromatographic method as well as by the high-pressure liquid chromatographic method. Good agreement was obtained between the 2 methods.

High-Pressure Liquid Chromatographic Method for the Determination of Patulin in Apple Butter

1975 ◽  
Vol 58 (4) ◽  
pp. 754-756 ◽  
Author(s):  
George M Ware
Keyword(s):  
High Pressure ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Chromatographic Method ◽  
High Pressure Liquid Chromatographic ◽  
Ultraviolet Detector ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract Patulin is extracted from apple butter samples with ethyl acetate and the extract is cleaned up on a silica gel column, using benzene-ethyl acetate (75+25) as the eluant. High-pressure liquid chromatography, using a 25 cm Zorbax-Sil column, isooctane-ethyl ether-acetic acid (750+250+0.5) as the mobile solvent, and a 254 nm ultraviolet detector, is used for the determinative step. Under these conditions, patulin is eluted before 5-hydroxymethylfurfural, a component of apple butter which interferes with other liquid chromatographic and thin layer chromatographic methods. Recoveries of patulin added at levels of 34.6, 138.4, and 276.8 μg/kg ranged from 89.0 to 112.1%.

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