Search

Arbutin is the main active ingredient in many herbal medicinal products that have diuretic, antimicrobial, bactericidal, and antioxidant effects. Many of these products are mixtures of different herbal substances. Therefore, the approaches to quality control of HMPs can vary significantly. The aim of the study was to compare arbutin assay procedures used in quality control of arbutin-containing products. Materials and methods. Samples of the following HMPs were used in the study: monocomponent Bearberry Leaf and multicomponent Brusniver® (herbal mixture, powder). The test methods used were titrimetry, ultraviolet-visible spectrophotometry, and high-performance liquid chromatography (HPLC). Results. The authors compared five arbutin assay procedures described in the monographs and product files for arbutin-containing HMPs. Conclusions. It has been established that the analysed procedures cannot be used interchangeably as equivalent test methods; the limits for arbutin have to be established for each specific procedure. Iodometric titration is the most labour- and time-consuming method, and the determined titration endpoint is a subjective assessment. Spectrophotometric methods do not require the use of an arbutin reference standard, but they can give overestimated results as compared to the HPLC and titrimetry methods. HPLC methods are more selective, but they require the use of reference standards. The recommended test methods for HMP quality control are HPLC and visible spectrophotometry; the titrimetric method is recommended for replacement.

Identification of hellebore (Veratrum Lobelianum Bernh.) herbal substance, as well as hellebore-based herbal preparation and herbal medicinal product by the same group of biologically active substances using the same test method is in line with the so-called “consistent standardisation” principle.The aim of the study was to develop a harmonised approach to identification of steroidal alkaloids in hellebore products (hellebore water, hellebore tincture) and hellebore herbal substance (hellebore rhizomes with roots).Materials and methods: samples of hellebore water, hellebore tincture, and hellebore rhizomes with roots were analysed by high-performance thin-layer chromatography (HPTLC) using an HPTLC plate.Results: the authors developed a harmonised identification procedure for products made from hellebore rhizomes with roots (herbal substance, herbal preparation, and herbal medicinal product) based on HPTLC detection of steroidal alkaloids. The results of the study will be used to prepare amendments to the Identification part of monograph FS.2.5.0104.18 “Hellebore rhizomes with roots”. The developed test procedure is proposed for inclusion into draft monographs “Hellebore rhizomes with roots, tincture” and “Hellebore rhizomes with roots, tincture, solution for external use”.Conclusions: the developed test procedure can be used as an identification test for a range of products from the hellebore herbal substance to hellebore-based herbal medicinal products, which is based on the detection of the same group of biologically active substances.

Papaverine hydrochloride products are used as anticonvulsants in routine medical practice. Most of the approved product specification files include thin-layer chromatography for assessment of product-related impurities and UV spectrophotometry for determination of active pharmaceutical ingredients. An HPLC assay is not used for determination of papaverine hydrochloride in drug dosage forms.The aim of the study was to develop an HPLC test method for determination of product-related impurities and for quantification of papaverine hydrochloride in solutions for injection, tablets, and rectal suppositories.Materials and methods: samples of the following Russian-made papaverine products were used in the study: Papaverine, solution for injection, 20 mg/mL; Papaverine, rectal suppositories, 20 mg; Papaverine, tablets, 40 mg. The Agilent 1260 Infinity II DAD System was used for the HPLC assay, and the Agilent 8453Е UV-Vis System was used for recording UV spectra. The determination of product-related impurities and the assay of active ingredients were performed simultaneously by HPLC using a reversed-phase column Kromasil 100-5-C18, 250×4.6 mm, 5 μm, the gradient elution mode, and detection at 238 nm. Papaverine Hydrochloride USP RS, 99% purity, and Noscapine EP CRS were used as reference standards.Results: the study demonstrated that determination of product-related impurities and assay of active ingredients in papaverine products can be performed simultaneously using HPLC.Conclusions: the authors proposed an HPLC test method for determination of active ingredients in papaverine products, which is aligned with the “consistent standardisation” principle and can be recommended for inclusion into draft monographs for papaverine products.

Specialists in pharmacognosy are facing an important task of improving quality control methods for combination herbal medicinal products in order to enable reliable assessment of the content of active substances that are responsible for the drug’s pharmacological effect.The aim of the study was to investigate the possibility of using the European Pharmacopoeia method to determine the total content of anthracene derivatives in the antihaemorrhoidal medicinal herb mixture Proctophytol® and to propose limit values for the total content of anthracene derivatives.Materials and methods: individual mixture components containing anthracene derivatives, such as senna leaves and frangula bark, as well as model mixtures containing these individual components in a 1:1 ratio, and a model mixture imitating Proctophytol® were used in the study. The determination of the anthracene derivatives content was carried out using spectrophotometry.Results: it was demonstrated that the European Pharmacopoeia method could be used to assess the quality of Proctophytol® in terms of anthracene derivatives total content. The spectrophotometric method described in the European Pharmacopoeia has advantages over the methods described in manufacturer specifications for Russian products, because it allows for thorough extraction of the active substances and is standardized for anthracene derivatives.Conclusions: the European Pharmacopoeia method was adjusted to determine anthracene derivatives in the medicinal herb mixture Proctophytol®. It was proposed to use 70% ethanol instead of 70% methanol as extraction solvent. The authors identified optimum sample weights and test solution dilutions, and calculated and verified the limit for anthracene derivatives content—“Not less than 1.9%”. The adjusted method can be recommended for inclusion in the monographs of the State Pharmacopoeia of the Russian Federation for medicinal herb mixtures similar to Proctophytol®.

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 objectiveof the studywas 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.

The article describes results of comparative evaluation of two pharmacopoeial methods used for quantitative determination of tannins in herbal drugs: the titrimetric method of the State Pharmacopoeia of the USSR (XIth edition) that is described in the draft general monograph «Determination of tannins in herbal drugs» to be included in the State Pharmacopoeia of the Russian Federation, XIII edition, and the spectrophotometric method of the European Pharmacopoeia. Basic metrological characteristics of the methods were determined using oak bark as sample herbal drug. Both methods were used to test the quality of 9 herbal drug samples in which tannins were present as the main group of biologically active substances. It was revealed that the determined amount of tannins depends on the method used; and content limits are different for the two methods. Experiments were undertaken with the addition of pyrogallol. A modification of the titrimetric method of the State Pharmacopoeia of the USSR (XIth edition) was considered with a view of increasing tannins yield from herbal drugs; conclusions were made regarding the need to change the tannins limit for the modified method.

The paper describes the basic quality parameters of the starting materials of herbal origin and herbal drugs, taking into account the requirements of State Pharmacopeia XI and draft general chapters of State Pharmacopeia XIII. It enlists the main terms and definitions, and the requirements to presentation of the quality parameters. It provides the examples of typical criticism of the normative documents on herbal drugs in terms of various quality parameters, including “Appearance”, “Identification tests”, “Chromatography”, “Degree of fineness”, “Assay”. The criticism has been leveled at the quality of both draft normative documents and the samples submitted for testing. The survey conducted allows for explaining the expert requirements to the quality of samples and the presentation of several test methods.

The article compares two methods of loss on drying determination in herbal medicinal products: drying using an infrared thermographic moisture analyzer and drying carried out in a drying cabinet. Data obtained with the moisture analyzer were shown to be sufficient for determination of loss on drying in herbal medicinal products of different morphological groups and were generally consistent with the data obtained by the traditional pharmacopoeial method - drying in a drying cabinet. The article demonstrates the feasibility of performing loss on drying test using an infrared thermographic moisture analyzer.

The review contains summary information about possible impurities, determination of which is described by draft monograph «fixed vegetable oils» and state standards of Russian Federation. The review briefly describes methods for determination of soaps, unsaponifiable components, residual solvents, volatile compounds, foreign fatty oils, aldehydes, moisture, proteins, paraffin, wax, tar and mineral oils, heavy metals, phosphorus-containing substances, cyanides and hydrogen cyanides.