Colorimetric determination of propoxur and its residues in vegetables

A method has been developed for the determination of propoxur (o-isopropoxyphenyl N-methylcarbamate) based on the hydrolysis of propoxur with methanolic potassium hydroxide to its phenol and coupling with diazotized 4,4-diaminodiphenyl sulfone. The orange complex formed has an absorption maximum at 500 nm and obeys Beer's law in the range 0.25-5.0 micrograms/mL. The method can be applied to levels as low as 0.5 ppm propoxur from vegetables.     

Colorimetric determination of alkaline phosphatase as indicator of mammalian feces in corn meal: collaborative study

In the official method for rodent filth in corn meal, filth and corn meal are separated in organic solvents, and particles are identified by the presence of hair and a mucous coating. The solvents are toxic, poor separation yields low recoveries, and fecal characteristics are rarely present on all fragments, especially on small particles. The official AOAC alkaline phosphatase test for mammalian feces, 44.181-44.184, has therefore been adapted to determine the presence of mammalian feces in corn meal. The enzyme cleaves phosphate radicals from a test indicator/substrate, phenolphthalein diphosphate. As free phenolphthalein accumulates, a pink-to-red color develops in the gelled test agar medium. In a collaborative study conducted to compare the proposed method with the official method for corn meal, 44.049, the proposed method yielded 45.5% higher recoveries than the official method. Repeatability and reproducibility for the official method were roughly 1.8 times more variable than for the proposed method. The method has been adopted official first action.     

Colorimetric determination of stanozolol in pharmaceutical formulations

In acidic medium, stanozolol reacts with phenoldisulfonic acid to form a stable yellow chromophore, which is quantitated by spectrophotometry at 385 nm. The reaction gives a linear response at concentrations from 5 to 50 micrograms/mL. The method is suitable for routine analytical control of stanozolol and its formulations.     

Colorimetric determination of arprinocid in feed.

An analytical method has been developed for the determination of arprinocid (9-(2-chloro-6-fluorophenylmethyl)-9H-purin-6-amine) in feed, based upon measurement of the absorbance of the diazo chromophore formed from a product of zinc reduction of the drug in acidic solution. The analyte is extracted from the feed into chloroform in the presence of a pH 7 phosphate buffer and isolated by adsorption chromatography on alumina, followed by partitioning between hexane and 0.15M HCl. The reduction product in the aqueous phase is then treated for colorimetric measurement. This procedure has been applied to determining 0.0010--0.0080% arprinocid in feed with a precision of less than 5% relative standard deviation near the middle of this concentration range. Of 32 feed additives examined, only zoalene and sulfamethazine were serious interferences. A study and discussion of several factors, e.g., reaction time, pH, and amount of zinc metal, that affect the analytical reactions are also included.     

Simultaneous determination of carbaryl, malathion, fenitrothion, and diazinon residues in sesame seeds (Sesamum indicum L.)

A method is described for the simultaneous determination of carbaryl (1-naphthyl methylcarbamate), malathion [diethyl (dimethoxythiophosphorylthio) succinate], fenitrothion (O,O-dimethyl O-4-nitro-m-tolyl phosphorothioate), and diazinon (O,O-diethyl O-2-isopropyl-6-methylpyrimidin-4-yl phosphorothioate) in sesame (Sesamum indicum L.) seeds. Sesame seeds were Soxhlet extracted with n-hexane, and the extract was subjected to a liquid-liquid partitioning and column cleanup to remove the oily coextractives prior to analysis by high performance liquid chromatography (HPLC). The mean percent recoveries (+/- standard deviations) from sesame seeds fortified with carbaryl (0.004 to 0.035 microgram/g), malathion (0.53 to 4.25 microgram/g), fenitrothion (0.22 to 1.78 microgram/g), and diazinon (0.54 to 4.35 microgram/g) were 83.3 +/- 5.7, 85.5 +/- 6.6, 85. 6 +/- 7.2, and 88.4 +/- 4.8, respectively. The method was used for the simultaneous analysis of carbaryl, malathion, fenitrothion, and diazinon residues in sesame seeds obtained from an Ethiopian field crop that had been treated with the pesticides during its growing period.     

Colorimetric determination of tetracycline hydrochloride in pharmaceutical preparations

A simple, sensitive, and rapid colorimetric method is presented for the estimation of tetracycline hydrochloride as the pure drug and in formulations. The proposed method is based on the reaction of tetracycline HCl with cupric chloride in an alkaline medium to give a yellowish green solution whose absorbance is measured at 400 nm against a reagent blank. The color obeys Beer's law in the concentration range of 0-20 micrograms/mL. Molar absorptivity and Sandell's sensitivity of the yellowish-green copper complexes of tetracycline HCl are 1.99 X 10(4) L X mol-1 X cm-1 and 0.0241 ppm, respectively.     

Colorimetric determination of tetracycline derivatives in pharmaceutical preparations

A quick colorimetric method is reported for the determination of tetracycline derivatives such as oxytetracycline hydrochloride (OTCH), chlortetracycline hydrochloride (CTCH), methacycline hydrochloride (MCH), and doxycycline hydrochloride (DCH). The method involves complexation of the above derivatives with cupric chloride in alkaline medium. The yellowish green copper complexes of OTCH, CTCH, MCH, and DCH show maximum absorbance at 395, 410, 400, and 400 nm, respectively. The color intensity obeys Beer's law in the concentration range of 0-20 micrograms/mL.     

Colorimetric determination of caffeic acid in plant materials

A new colorimetric method is described for determining caffeic acid content in plant materials. Caffeic acid is separated by thin layer chromatography from the alcoholic extract, and color is developed using 0.5% aqueous thiosemicarbazide solution under alkaline conditions. The absorbance is read at 475 nm. Lambert-Beer's law is obeyed in the concentration range 0.37-17.5 micrograms caffeic acid/mL. The method is reproducible and has been applied to the estimation of caffeic acid in carrot roots.     

Colorimetric determination of diazepam in pharmaceutical preparations.

A colorimetric method is presented for the estimation of diazepam as the pure drug and in formulations. Diazepam is hydrolyzed with 6N HCl to 2-methylamino-5-chlorobenzophenone, which is extracted with chloroform to give a yellow solution whose absorbance is measured at 410 nm against a solvent blank. The color obeys Beer's law in the concentration range of 0-30 mug/ml. In 5 determinations, recovery was 99.0 +/- 1.9%. The method is applicable to pure diazepam and its formulations for oral and parenteral use. No interferences were observed from pyridoxine hydrochloride and commonly used preservatives, vehicles, and colors.     

Colorimetric determination of hydralazine with 9-chloroacridine

A spectrophotometric assay for hydralazine hydrochloride based on the interaction of the drug with 9-chloroacridine has been developed. The interaction shows an absorption maximum at 460 nm and is affected by temperature, heating time, and quantity of acridine reagent used. Color development is maximum when the drug is heated in the presence of a 30-fold molar excess of the acridine in a 50 +/- 1 degree C water bath for 1 hr. The method detects hydralazine hydrochloride in the 10(-5)--10(-6)M range with sensitivity to 0.2 micrograms/mL and 3--4% accuracy. Typical calibration data obtained from linear regression analysis of absorbance at various drug concentrations show r = 0.9997 (n = 6). Hydralazine can be determined in dosage forms that also contain varying quantities of reserpine and hydrochlorothiazide. The 9-chloroacridine method is as sensitive as other spectrophotometric procedures for hydralazine but also more accurate and precise, and involves fewer manipulative steps.     

Colorimetric method for the determination of lipoxygenase activity

A colorimetic assay for lipoxygenase activity has been developed. The assay is based on the detection of the lipoxygenase reaction product, linoleic acid hydroperoxide, by the oxidative coupling of 3-methyl-2-benzothiazolinone (MBTH) with 3-(dimethylamino)benzoic acid (DMAB) in a hemoglobin-catalyzed reaction. This test reaction is rapid and sensitive, and it offers advantages over other methods for detecting lipoxygenase activity. The assay is capable of detecting activity in a number of crude vegetable homogenates and should be particularly useful where a rapid visual determination of lipoxygenase activity is desired.     

Colorimetric determination of sympathomimetic amines methyldopa and noradrenaline

The chromogenic reagent p-dimethylaminocinnamaldehyde (PDAC) is introduced for the determination of the sympathomimetic amines methyldopa and noradrenaline. The method is based on measurement of the orange color developed when the alkaline solution of methyldopa and noradrenaline is allowed to react with PDAC at pH 5.0. The color developed obeys Beer's law in the concentration range 0.1-1.5 mL of 2 X 10(-3)M solution of noradrenaline and methyldopa. The results are compared with those obtained with another chromogenic reagent, p-dimethylaminobenzaldehyde (PDAB). Determinations on dosage forms of the drugs, using PDAC and PDAB reagents, agreed well with results of determinations by official pharmacopoeial methods.     

Colorimetric method for field-screening above-tolerance parathion residues on and in citrus fruits

A colorimetric technique has been developed which is suitable for use as a field-screening method for detecting above-tolerance levels of parathion on and in citrus fruits. By using this method, a grower should be able to postpone harvesting a crop until parathion residues are below tolerance level, so that the crop is safe to market. The method depends on the reaction of parathion with 4-(p-nitrobenzyl)-pyridine. Parathion is extracted by mixing chopped citrus rind with acetone in a hand-operated homogenizer. The extract is partially cleaned by a partitioning step before final cleanup with a Sep-Pak Florisil cartridge. The colored reaction solution is read at 560 nm by using a portable, rechargeable spectrophotometer. A single test can be completed in about 75 min; the average time per test when several are conducted sequentially is considerably shorter. The analytical system responds readily to less than 5 ppm parathion on or in 1 g navel orange rind, which corresponds to less than 1 ppm in the whole fruit. The present U.S. tolerance for parathion on or in citrus is 1 ppm on a whole fruit basis. Preliminary work indicates that the method should also be suitable for apples.     

Colorimetric determination of mestranol in combination with ethynodiol diacetate.

Mestranol in combination with ethynodiol diacetate, an oral contraceptive formulation, is isolated from the sample on a partition chromatographic column prior to colorimetric determination. The color reaction which is specific for estrogens is formed by shaking an aliquot of the heptane eluate of mestranol with a 30% methanol-sulfuric acid solution. A collaborative study of the method gave results of 99.8% of added mestranol for the simulated mix and 100.7% of labelled mestranol for the commercial tablet. The method has been adopted as official first aciton.