Acetaminophen Acetaminophen is an analgesic and an antipyretic, but the exact mechanism of the drug action is not fully understood. It appears to relieve pain by raising the pain threshold so that a greater amount of pain is necessary before it can be felt. Its antipyretic action results from its effect on the heat-regulating centers of the brain. Chemically, acetaminophen is p-hydroxy acetanilide, it has a molecular weight of 151.16 and elemental analysis shows it contains 67.38% carbon, 9.43% hydrogen, 5.24% nitrogen and 17.95% oxygen. Acetaminophen is prescribed for arthritis but is not an anti-inflammatory, it is mainly used to help reduce temperature and as a mild analgesic. Acetaminophen tablets have been successfully analyzed using reversed phase (C18) columns 20-25 cm long 3-4.6 mm in diameter using a strongly polar, water-methanol-acetonitrile mixture with a tetramethylammonium hydroxide buffer as the mobile phase. By employing a C18 stationary phase strong dispersive interactions are exploited in the stationary phase whereas predominantly polar interactions are active in the mobile phase. Separations can be easily obtained in 5 to 10 minutes

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Author: RPW Scott Book:Principles and Practice of Chromatography
Section:Principles   Applications   Liquid-Chromatography

(adjusted to pH 7 with 85% phosphoric acid)60% acetonitrile and 15% methanol Flow-Rate 2 ml/min. Detector UV adsorption at 215 nm Sample Volume 100ml     An example of the use of native silica is in the analysis of Darvocet® and its generic equivalent formulation. The separation obtained is shown in figure 44. Darvocet® is an acetaminophen product of which acetaminophen itself is the active ingredient together with other weakly polar substances present. Consequently, the mixture lends itself to separation on silica gel. The analysis was completed in less than 4 minutes using a short column 3.3 cm long and 4.6 mm in diameter. The silica packing had a particle size of 3 m providing a maximum efficiency of about 5,500 theoretical plates.   Courtesy of Supelco Inc.   Figure 44 The Analysis of Acetaminophen Formulations

Principles   Applications   Liquid-Chromatography

Author: RPW Scott Book:Principles and Practice of Chromatography
Section:Principles   Selectivity   Polar

An interesting example of polar selectivity by hydroxyl groups on the surface of native silica is shown by the analysis of Darvocet® and its generic equivalent in figure 15. Courtesy of Supelco Inc. Figure 15 The Analysis of Acetaminophen Formulations   Darvocet® is an acetaminophen product in which it is the active ingredient. Other substances are present which also contain polar groups and thus, the sample lends itself to separation on the polar stationary phase, silica gel. The analysis was completed in less than 4 minutes using a short column 3.3 cm long and 4.6 mm in diameter packed with silica (particle size of 3 m). The column appears to be significantly overloaded, but the impurities are

Principles   Selectivity   Polar

Author: RPW Scott Book:Liquid Chromatography
Section:HPLC   Applications

was shown to be present in the generic formulation that was not in the Darvocet®. The mobile phase was 98.5% dichloromethane with 1.5% v/v of methanol containing 3.3% ammonium hydroxide. The ammoniacal methanol deactivated the silica gel but the interaction of the solutes with the stationary phase would still be polar in nature. In contrast solute interactions with the methylene dichloride would be exclusively dispersive.   Courtesy of Supelco Inc.   Figure 59. The Analysis of Acetaminophen Formulations   Ion chromatography can be used in a number of novel ways and employing the appropriate conditions can even be used to separate mixtures where the components are not ionic or do not normally  produce interactive ions in aqueous solution. An example of this type of separation is the analysis of saccharide mixtures using ion exchange interactions. An illustration of such a separation is given in figure 60. The  saccharides are reacted with a borate with which

HPLC   Applications

Author: RPW Scott Book:Liquid Chromatography
Section:HPLC   Applications

the stationary phase would become almost exclusively dispersive. This is an example where a complex phase system was necessary because there was limited column efficiency available. It is likely that a column with intrinsically more efficiency might achieve the separation with a much simpler solvent system and a more straightforward solvent program. An example of the use of native silica is given by for the analysis of Darvocet® and its generic equivalent formulation. Darvocet® is an acetaminophen product in which the active ingredient (and other material in the medicine) are weakly polar and, consequently, lend themselves to separation on a strongly polar stationary phase such as silica gel. The analysis is depicted in figure 59. The analysis is completed in less than 4 minutes using a short column 3.3 cm long and 4.6 mm in diameter. The silica packing had a particle size of 3 m providing a maximum efficiency of about 5,500 theoretical plates

HPLC   Applications

 
 
 

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