scholarly journals Modification and validation of the test procedure for determination of sub-visible particulate matter in parenteral solutions, using the Coulter method

2021 ◽  
Vol 21 (2) ◽  
pp. 108-115
Author(s):  
A. A. Voropaev ◽  
O. V. Fadeikina ◽  
D. S. Davydov ◽  
A. A. Movsesyants
Keyword(s):  
Particulate Matter ◽  
Particle Concentration ◽  
Test Procedure ◽  
Particle Sizes ◽  
Reference Standard ◽  
Light Obscuration ◽  
Visible Particle ◽  
Modified Test ◽  
Count Reference

The State Pharmacopoeia of the Russian Federation, 14th edition provides for determination of sub-visible particles (less than 100 µm in size) in parenteral dosage forms using the Coulter method, in addition to the light obscuration particle count test and microscopy. However, the proposed 100 µm aperture tube does not enable assessment of the whole range of sub-visible particle sizes. Therefore, research is needed to find optimal test conditions for determination of sub-visible particulate matter by the Coulter method. The aim of the study: modification of the Coulter-based procedure using a 200 µm aperture tube, and performance of validation studies. Materials and methods: Multisizer 4e Coulter counter, suspensions of reference latex particles (10 µm, 20 µm, and 43 µm), and a particulate count reference standard containing 0.998 × 106 particles/mL were used in the study. The following parameters were assessed during validation: accuracy, repeatability, linearity. Results: the study confirmed the feasibility of using the modified Coulter-based procedure with a 200 µm aperture tube. The following values were obtained during validation of the modified test procedure: accuracy was 5.3% (deviation from the mean value) as compared to the particulate count reference standard, and 4.2% as compared to the light obscuration method. Repeatability was 1% (relative standard deviation) for the particle concentration of approximately 10000 per 1 mL, and 7.6% for the particle concentration of approximately 300 per 1 mL. The study demonstrated the linearity of the procedure, the linear correlation coefficient was more than 0.99. Conclusions: the studied validation parameters of the modified test procedure were shown to comply with the acceptance criteria. The modified test procedure will enable assessment of the whole range of sub-visible particle sizes when testing parenteral solutions for particulate contamination: sub-visible particles.

Case Study on Determination of Tensile Properties of Construction Sealants at Variable Temperatures

2016 ◽  
Vol 824 ◽  
pp. 18-26 ◽  
Author(s):  
Barbora Nečasová ◽  
Pavel Liška ◽  
Jiří Šlanhof ◽  
Martina Šimáčková
Keyword(s):  
High Temperature ◽  
Porous Materials ◽  
Tensile Properties ◽  
Test Procedure ◽  
European Standard ◽  
Specific Material ◽  
Modified Test

The authors of presented research case focused on possibilities of sealing porous as well as non – porous materials and analysed the measured results. It is the second article of the above mentioned authors dealing with sealed joints, however, in this case study the focus was placed on a group of industrially manufactured modified silyl polymer and polyurethane sealants. The research is based on the modified test procedure for the determination of adhesion and cohesion properties during maintained extension at variable temperatures, i.e. a high temperature of (70 + 2) °C and a temperature simulating freezing, i.e. (-20 + 2) °C, according to the European standard EN ISO 9047. The degree of specimen extension was set to amplitude of 20.0 % and the aim of the research case was to discover any differences that might appear in the resistance. The measured results demonstrate that there are significant differences between individual sealants in the results they provide in combination with specific material, e.g. wood appears to be a problematic substrate as well as glass cement or aluminium.

scholarly journals Evaluation of the Stability of Performance of the Analytical Test Method Used for Determination of Anticomplementary Activity of Human Immunoglobulin Preparations

2019 ◽  
Vol 19 (2) ◽  
pp. 118-123
Author(s):  
O. G. Kornilova ◽  
E. A. Khusnatdinova ◽  
E. S. Konovalova ◽  
R. A. Volkova
Keyword(s):  
Quality Control ◽  
Control Charts ◽  
Test Procedure ◽  
Human Immunoglobulin ◽  
Analytical Performance ◽  
Reference Standard ◽  
Anticomplementary Activity ◽  
Immunoglobulin Preparations ◽  
The Stability

The evaluation of anticomplementary activity, being an obligatory component of the quality control ofhuman immunoglobulin preparations, requires the use of a number of reagents of biological origin that are difficult to standardise. In order to standardise the quality control method used for determination of antiсomplementary activity it is advisable to use a reference standard which demonstrates whether obtained results comply with the acceptance criteria, and helps to assess the stability of analytical performance. The aim of the study was to assess the stability of analytical performance of the test procedure used for determination of antiсomplementary activity of human immunoglobulin preparations using human immunoglobulin reference standards of various grades. Materials and methods: anticomplementary activity was determined by the complement fixation test in accordance with the general monograph of the State Pharmacopoeia of the Russian Federation (14th ed.) OFS.1.8.2.0007.15 using different batches of guinea pig complement and sheep red blood cells. The test procedure was standardised using the OSO 42-28-430-2018 human immunoglobulin reference standard and the human immunoglobulin BRP, batch 1 (cat. No. Y0001504). The obtained results of anticomplementary activity of the reference standards were used to construct Shewhart control charts, using the certified values as control limits. Results: the analysis of the constructed Shewhart charts helped to assess trends, and estimate the influence of different batches of guinea pig complement and sheep red blood cells on the stability of analytical performance of the test procedure used for determination of antiсomplementary activity of human immunoglobulin preparations. Conclusions: the use of the OSO 42-28-430-2018 reference standard in combination with Shewhart control charts for the quality control of human immunoglobulin preparations in terms of Anticomplementary activity makes it possible to control the testing process, and assess any of its changes associated with the replacement of the batch of the reagent. At the same time, the reference standard of the European Pharmacopoeia, which has a wide range of permissible values, can only be used to confirm the acceptance of the results. Further studies to determine the mean value of the anticomplementary activity of control samples, as well as the standard deviation, may increase the possibilities of using this reference standard for assessment of analytical performance stability.

scholarly journals Current Approaches to Valerian Tincture Standardisation in Terms of Assay

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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