Quantitative Determination of Urinary Indoxyl Sulphate (Indican) and the Total Content of Basic Compounds in the Faeces of Cattle in Relation to Hypomagnesaemia

The process of harmonisation of Russian and foreign approaches and requirements in the field of medicines quality assurance calls for revision of quality control procedures included in various regulations and guidelines. The monograph FS.2.5.0062.18 “Hawthorn flowers” of the State Pharmacopoeia of the Russian Federation XIV edition includes a test procedure for determination of flavonoids by a chromatospectrophotometric method. This procedure does not take into account current scientific capabilities and has a number of shortcomings, therefore it was necessary to revise the existing test procedure and develop a new approach to the standardisation of the hawthorn flower herbal substance.The objective of the study was to develop an assay method for standardisation and evaluation of hawthorn flower using high performance liquid chromatography (HPLC).Materials and methods: the study was performed using samples of hawthorn flowers by Russian manufacturers. Quercetin (USP RS) and Hyperoside (HWI, primary standard) were used as the reference standards. The HPLC analysis was performed using an Infinity II 1260 DAD LC system (Agilent), and the UV spectra were recorded on a Cary 100 Varian spectrophotometer. A TLC Visualizer (CAMAG) was used to obtain digital images of thin layer chromatography plates.Results: the authors developed an HPLC test procedure for quantitative determination of total flavonoids, expressed as hyperoside, in hawthorn flowers. The developed procedure gives reliable and reproducible results and is characterised by high sensitivity and selectivity. The results of quantitative determination of the total flavonoid content in hawthorn flowers were used to propose the standard for the total content of flavonoids, expressed as hyperoside, of “not less than 0.5%”.Conclusions: the developed assay method for determination of active pharmaceutical ingredients in hawthorn flower products by HPLC can be recommended for inclusion into the Assay part of the “Hawthorn Flowers” monograph of the State Pharmacopoeia of the Russian Federation.

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Current Approaches to Valerian Tincture Standardisation in Terms of Assay

The Bulletin of the Scientific Centre for Expert Evaluation of Medicinal Products ◽

10.30895/1991-2919-2019-9-4-265-271 ◽

2019 ◽

Vol 9 (4) ◽

pp. 265-271

Author(s):

N. P. Antonova ◽

E. P. Shefer ◽

A. M. Kalinin ◽

N. E. Semenova ◽

S. S. Prokhvatilova ◽

...

Keyword(s):

Quantitative Analysis ◽

Quantitative Determination ◽

High Performance ◽

Test Procedure ◽

Total Content ◽

Reference Standard ◽

Active Ingredients ◽

Test Procedures ◽

Valerenic Acid

The quality control of the «Valerian rhizome and roots» herbal substance is carried out using high performance liquid chromatography (HPLC) according to the State Pharmacopoeia of the Russian Federation, XIV edition. The quantitative analysis of the active ingredients in valerian tincture is performed using a non-specific and non-selective spectrophotometric method. Therefore, it is important to introduce in Russia a more modern test procedure for quantitative determination of active ingredients in valerian tincture.The aim of the study was to develop a selective and sensitive HPLC procedure for quantitative determination of the total content of sesquiterpenic acids, expressed as valerenic acid, for the purpose of valerian tincture standardisation.Materials and methods: valerian tincture samples produced by seven Russian manufacturers were used as test samples, and valerenic acid was used as the reference standard. The quantitative analysis of the active ingredients was performed by two methods: spectrophotometry at 512 nm following the reaction of valerenic acid ethylester with hydroxyalamine and ferric chloride, and by HPLC using a Nucleosil C18 column, 125×4.6 mm, 5 µm particle size, in gradient elution mode, with detection at 220 nm.Results: the spectrophotometric technique was shown to be insufficiently specific. The authors of the study validated the chromatographic test procedure, established system suitability criteria, and compared the results obtained by the two test procedures. They also determined a tentative standard of the total content of sesquiterpenic acids, expressed as valerenic acid, obtained by HPLC.Conclusions: the HPLC assay developed for quantitative determination of active ingredients in valerian tincture is more specific as compared to the spectrophotometric technique, as the sum of the peaks of valerenic and acetoxyvalerenic acids and the results for the reference standard are taken into account during calculations. The new test procedure is in line with the cross-cutting standardisation principle and can be recommended for inclusion into the draft monograph «Valerian tincture».

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Quantitative determination of the total content of flavonoids in a cholagogic species

Pharmaceutical Chemistry Journal ◽

10.1007/bf02508454 ◽

1999 ◽

Vol 33 (3) ◽

pp. 151-154

Author(s):

L. P. Smirnova ◽

L. N. Pervykh

Keyword(s):

Quantitative Determination ◽

Total Content

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QUANTITATIVE DETERMINATION OF IODOAMINO ACIDS IN THE THYROID GLAND OF THE PARROT-FISH (SCARUS GUACAMAIA)

Journal of Endocrinology ◽

10.1677/joe.0.0460417 ◽

1970 ◽

Vol 46 (4) ◽

pp. 417-423 ◽

Cited By ~ 5

Author(s):

A. J. MATTY ◽

C. C. THORNBURN

Keyword(s):

Body Weight ◽

Quantitative Analysis ◽

Thyroid Gland ◽

Quantitative Determination ◽

Sex Difference ◽

Total Content ◽

Parrot Fish

SUMMARY A quantitative analysis of the iodoamino acids in whole dried parrot-fish thyroid gland was carried out by determination of stable 127I. Mono- and di-iodotyrosine together made up about half of the total iodoamino acids and thyroxine about a third to a half. The tri-iodothyronine content was low, about 5%. The total content of the acids increased with body weight, and there was an indication of a sex difference.

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