РАЗРАБОТКА ИК-СПЕКТРОМЕТРИЧЕСКОЙ МЕТОДИКИ ОПРЕДЕЛЕНИЯ АНТИОКИСЛИТЕЛЬНОЙ ПРИСАДКИ АГИДОЛ-1 В РАСТВОРАХ, ИСПОЛЬЗУЕМЫХ ДЛЯ ВВЕДЕНИЯ ЕЁ В ДИЗЕЛЬНОЕ ТОПЛИВО

The rapid infrared spectrometric technique was developed and introduced in the analytical laboratory at the plant for the determination of antioxidant additive Agidol-1 inconcentrated solutions used for the introduction of this additive to diesel fuel. The optimum conditions were selected for the sample preparation for an analysis. The metrological characteristics of the developed technique were evaluated such as the repeatability (Vr) and interlaboratory precision (VRl) which are characterized by the coefficients of variation 0.31 and 0.24% respectively; the systematic error, determined by use of the model samples, is negligible. The analysis of one sample takes 15-20 minutes after its delivery to the laboratory. The potentiometric technique, earlier used to control the content of additive Agidol-1, is characterized by Vr = 2.57 and VRl = 2.87%; the sample is analyzed about 1.5 days. There is significant systematic disagreement between the results of the sample analyses using the developed and the earlier applied techniques.Key words: antioxidant additive Agidol-1, infrared spectrometric technique, repeatability, interlaboratory precision, systematic error(Russian)DOI: http://dx.doi.org/10.15826/analitika.2013.17.3.012E.V. Kaz'mina1, А.N. Smagunova1, N.P. Butina2, E.N. Korzhova1 1Irkutsk State University, Irkutsk, Russian Federation2Angarsk petrochemical company, Irkutsk Region, Russian FederationРазработана и внедрена в аналитическую практику предприятия экспрессная ИК-спектрометрическая методика определения антиокислительной присадки Агидол-1 в растворах-концентратах, используемых для введения этой присадки в дизельное топливо. Выбраны оптимальные условия подготовки проб к анализу. Оценены метрологические характеристики разработанной методики: повторяемость (Vr) и внутрилабораторная прецизионность (VRл) характеризуются коэффициентами вариации 0.31 и 0.24 % соответственно; систематическая погрешность, выявляемая с помощью модельных образцов, незначима. На анализ одной пробы от времени поступления её в лабораторию требуется 15-20 мин. Ранее используемая для контроля содержания присадки Агидол-1 потенциометрическая методика характеризуется Vr  = 2.57 и VRл = 2.87 %; длительность анализа пробы составляет около 1.5 суток. Между результатами анализа проб разработанной методикой и ранее используемой имеет место значимое систематическое расхождение.Ключевые слова:антиокислительная присадка Агидол-1, ИК-спектрометрическая методика, повторяемость, внутрилабораторая прецизионность, систематическая погрешность DOI: http://dx.doi.org/10.15826/analitika.2013.17.3.012 Литература1. Электрохимическое определение синтетических антиоксидантов – бисдитиофосфоновых кислот / Г.К. Зиятдинова и [др.] // Ж. аналит. химии. 2010. Т. 65, № 12. С. 1302-1308.2. РД 34.43.105-89. Методические указания по эксплуатации трансформаторных масел. М.: ПО «Союзтехэнерго», 1989. 45 с. 3. РД 34.43.208-95. Методика количественного химического анализа. Определение содержания присадок в энергетических маслах методом высокоэффективной жидкостной хроматографии. М.: РАО «ЕЭС России», 1995. 6 с.4. Применение микроколоночной ВЭЖХ для контроля ионола в трансформаторном масле / О.Б. Рудаков и [др.] // Сорбционные и хроматограф. процессы. 2008. Т. 8, Вып. 1. С. 141-146.5. РД 34.43.209-97. Экспресс-метод определения антиокислительной присадки (ионола) в свежих и эксплуатационных турбинных маслах М.: РАО «ЕЭС России», 1997. 4 с.6. Определение антиоксидантов ионола (2,6-дитретбутил-4-метил-фенола) в трансформаторных маслах кинетическим методом и методом ИК-спектроскопии / С.И. Писарева и [др.] // Ж.. аналит. химии. 2001. Т. 56, № 10. С. 1106-1109.7. ГОСТ Р 52368-2005 (ЕН 590:2009). Топливо дизельное ЕВРО. Технические условии. М.: Стандартинформ, 2005. 28 с. 8. Методика 1110-2011 ОАО АНХК. Присадки к топливам к маслам. Определение массовой доли нафтеновых кислот и Агидола-1 потенциометрическим титрованием в неводной среде. Ангарск: ОАО АНХК, 2011. 23 с.9. Смагунова А.Н., Карпукова О.М. Методы математической статистики в аналитической химии: учебное пособие. Ростов-на-Дону: Феникс, 2012. 346 с.10. РМГ 61-2003. Государственная система обеспечения единства измерений. Показатели точности, правильности, прецизионности методик количественного химического анализа. Методы оценки. М.: Изд-во стандартов, 2004. 42 с.11. Сопоставление метрологических характеристик прецизионности методик количественного химического анализа / А.Н. Смагунова и [др.] // Заводская лаборатория. Диагностика материалов. 2007. Т. 73, № 6. С. 68-72. 12. Каплан Б.Я., Филимонов Л.Н., Майоров И.А. Метрология аналитического контроля в цветной металлургии. М.: Металлургия, 1989. 200 с.13. Смагунова А.Н. Способы оценки правильности результатов анализа // Ж. аналит. химии. 1997. Т. 52, № 10. С. 1022-1029

Assessment of the Severity of Breast Artery Calcification on a Mammogram: Intraoperator and Interoperator Reproducibility

Purpose. To study approaches to the quantitative assessment of breast arterial calcification (BAC) – a new surrogate marker of high cardiovascular risk in women, to determine the most detailed way to quantify BAC and to assess the reproducibility of these parameters.Material and methods. Mammograms of 1,078 women were analyzed for the presence of BAC. The intraoperator reproducibility of the assessment of the severity of BAC using a 12-point scale (Margolies L et al., 2016) was studied by analyzing 20 mammograms by the same operator twice with an interval of at least 2 weeks. Inter-operator reproducibility was studied by analyzing 99 mammograms by two independent operators.Results. When assessing the intraoperative reproducibility of the total score for each mammary gland, the exact coincidence of the results was noted in 70% (95% confidence interval [CI] 53.5-83.4), in cases of difference of no more than 1 point – in 27.5% (95%CI 14.6-43.9), only in 1 case the difference in assessments was 2 points. No systematic error was found between the two measurements (p=1.0), the correlation coefficient was rs=0.973. The assessment of inter-operator reproducibility showed that the exact coincidence of indicators was present in 48.5% (95%CI 41.3-55.7), in 91.4% (95% CI 86.6-94.9) cases, the total score for each the mammary gland differed by no more than 1 point. There was no systematic error between the measurements of the two experts (p=0.438), the correlation coefficient was rs=0.942.Conclusion. A good intraoperator and interoperator reproducibility of indicators of the severity of BAC on a 12-point scale has been shown, which makes it possible to recommend it for use in science and practice

Prevalence and Severity of Breast Arterial Calcification on Routine Mammography

Aim. To determine the frequency of detection and severity of breast arterial calcification (BAC) among women undergoing mammography on the basis of medical institutions in Moscow.Material and methods. The analysis included 4274 digital mammograms of women aged 40-93 who underwent preventive or diagnostic mammography. Standard full-format digital mammograms were performed in craniocaudal and mediolateral oblique projections. In addition to the standard diagnosis of breast disease, all mammograms were evaluated for the presence of BAC. The severity of BAC was assessed on a 12-point scale: mild 3-4 points, moderate 5-6 points, severe 7-12 points.Results. The average frequency of BAC was 10.1%, in the middle age group 50-59 years – 6.0%. The incidence of BAC increased with age, from 0.4% to 0.6% in women <50 years of age to >50% in women ≥80 years of age. A statistically significant and pronounced correlation was found between the woman's age and the presence of BAC r Pearson =0.769 (p<0.001). There was also a less noticeable but statistically significant correlation between age and severity of BAC r Spearman =0.319 (p<0.001). Regression analysis made it possible to estimate the probability of CAD depending on age. In women <50 years of age, only mild to moderate calcification occurred, while those ≥65 years of age had a significant increase in the incidence of severe CAD.Conclusion. There was an expected increase with age in both prevalence and severity of BAC. Cases of severe BAC in women younger than 65 years of age and any BAC in women younger than 50 years of age are atypical and require clarification of their association with cardiovascular and other diseases

Viral ecogenomics across the Porifera

BackgroundViruses directly affect the most important biological processes in the ocean via their regulation of prokaryotic and eukaryotic populations. Marine sponges form stable symbiotic partnerships with a wide diversity of microorganisms and this high symbiont complexity makes them an ideal model for studying viral ecology. Here, we used morphological and molecular approaches to illuminate the diversity and function of viruses inhabiting nine sponge species from the Great Barrier Reef and seven from the Red Sea.ResultsViromic sequencing revealed host-specific and site-specific patterns in the viral assemblages, with all sponge species dominated by the bacteriophage order Caudovirales but also containing variable representation from the nucleocytoplasmic large DNA virus families Mimiviridae, Marseilleviridae, Phycodnaviridae, Ascoviridae, Iridoviridae, Asfarviridae and Poxviridae. Whilst core viral functions related to replication, infection and structure were largely consistent across the sponge viromes, functional profiles varied significantly between species and sites largely due to differential representation of putative auxiliary metabolic genes (AMGs) and accessory genes, including those associated with herbicide resistance, heavy metal resistance and nylon degradation. Furthermore, putative AMGs varied with the composition and abundance of the sponge-associated microbiome. For instance, genes associated with antimicrobial activity were enriched in low microbial abundance sponges, genes associated with nitrogen metabolism were enriched in high microbial abundance sponges and genes related to cellulose biosynthesis were enriched in species that host photosynthetic symbionts.ConclusionsOur results highlight the diverse functional roles that viruses can play in marine sponges and are consistent with our current understanding of sponge ecology. Differential representation of putative viral AMGs and accessory genes across sponge species illustrate the diverse suite of beneficial roles viruses can play in the functional ecology of these complex reef holobionts

Comparative-Legal Analysis of the Institute of Propietary Protectionin the Russian and Foreign Civil Law

In this article, a comparative legal analysis is conducted of the institution of proprietary protection in Russia and foreign countries. In particular, certain provisions of the civil legislation of such states as Germany, France, Austria, Italy, Switzerland, Netherlands, Portugal and England have been explored. Along with the study of foreign legal systems, the prospects for regulating proprietary protection in the rules of Russian civil law are examined on the basis of a detailed analysis of the Concept of the Development of Civil Legislation of the Russian Federation and the draft of Federal Law No. 47538-6 “On Amendments to Parts One, Two, Three and Four of the Civil Code of the Russian Federation, as well as in certain legislative acts of the Russian Federation”. The authors consistently disclose the content of the rules on property claims, the delineation of the approach to protecting the proprietary of movable and immovable things, the possibility of investigating the legal basis of possession within the possessory process, as well as the limits of self-defense of possession. As a result of the conducted research, the authors concluded that it is necessary to secure the proprietary protection in the norms of the current Russian legislation after the elimination of the indicated gaps and contradictions

The Value of Subclinical Carotid Atherosclerosis for Primary Prevention of Cardiovascular Diseases. Review of the Main International Studies

Measures for the prevention of cardiovascular diseases (CVD) are more effective if they are performed taking into account the risk factors of their development. Screening scales, which are helpful in determining the population risk, are used in primary prevention for cardiovascular (CV) risk stratification. The assessment of individual CV risk remains a problem. Biomarkers and instrumental investigations are used for its detailing. Carotid ultrasound is the main noninvasive method of vascular assessment. It allows assessing the intima-media thickness (IMT) and detecting the presence, location and morphology of atherosclerotic plaques (ASP), in other words, subclinical signs of atherosclerosis. Different views on the diagnosis of IMT and ASP in the carotid arteries and their value as predictors of CV and cerebrovascular diseases among individuals without CVD are presented in the article. Opinions about the benefits of IMT assessment for re-classification of patients with signs of subclinical atherosclerosis are also presented. The debate about the value of IMT in the CV risk stratification, and the feasibility of its assessment in clinical practice has not yet been completed. Assessment of IMT for CV risk stratification is most appropriate in patients with intermediate risk or with multiple risk factors of CVD. Consensus on primary CV prevention strategies in patients with intermediate risk of CVD is currently unavailable. Assessment of subclinical atherosclerosis by carotid ultrasound is important in such patients. The finding of increased carotid IMT should have an effect on the choice of hypolipidemic drug and intensity of treatment. However, the diagnosis of subclinical atherosclerosis is not built into the algorithm for determining the CV risk. This causes difficulties in choosing tactic of prophylactic intervention, especially for intermediate risk patients

Statins and the risk of cataract

Statins are one of the most commonly prescribed classes of drugs for the cardiovascular disease prevention and the treatment of hyperlipidemia. In the literature there is information about the association of statin taking and higher cataract risk. At the same time, there are studies that describe the protective effect of statins on cataracts. Due to the fact that with age the risk cataract increases, as does the likelihood of prescribing statins, the problem of side effects with its use is of particular importance. Despite the conflicting results, many authors agree that there is no convincing reason for statin refuse, since the advantages in cardiovascular risk reducing far outweigh the cataract risk and the possible need for its surgical treatment. The study presents 2 systematic reviews and 3 meta-analyzes about association of statin intake and cataract risk or its surgical treatment, as well as studies carried out over the past 5 years

DEVELOPMENT AND VALIDATION OF METHOD OF QUANTITATIVE DETERMINATION OF RESIDUAL ORGANIC SOLVENTS IN INNOVATIVE ACTIVE PHARMACEUTICAL INGREDIENT WITH GC-FID

The aim of the study was to develop and validate a new method of quantitative determination of residual organic solvents in a substance A using GLC. Studies were carried out with gas chromatography with a flame ionization detector and sampling from the vapor phase. The effect of the polarity of the stationary phase for the chromatographic separation of the organic solvents peaks: Chloroform, Ethanol, Methylene Chloride, Cyclohexane, Ethyl Acetate, Methanol, N, N-dimethylformamide, 2-propanol was investigated. Chromatographic separation of Ethanol, Methanol, 2-propanol, Ethyl Acetate, Methylene Chloride and Cyclohexane was performed with quartz capillary column DB-624, 30 m × 0.20 mm, 1.8 micron; Chloroform and N, N-dimethylformamide – DB-WAX, 30 m × 0.50 mm, 0.25 mm. System suitability criteria and the validity of method were determined. Method has high specificity, precision, linearity, sensitivity and reliability

SEVERAL ASPECTS OF DILTIAZEM AND ORGANIC NITRATES USAGE IN VARIOUS SEVERITY STABLE ANGINA PATIENTS

Aim. To estimate the effectiveness of Diltiazem (Dlt) and its combination with nitrates in patients with ischemic heart disease (CHD) and arterial hypertension (AH) according to exercise tolerance by functional class (FC) of stable angina (StA).Material and methods. 30 CHD male patients at the age of 58,8±7,5 with StA II FC (n=11), III FC (n=19) and 1–2 stage AH were included into open randomized placebo-controlled study. Drug therapy: Dlt 90–180 mg bid, isosorbide 5-mononitrate 50 mg qd, trinitrolong 2 mg bid or tid. Effectiveness of the regular drug intake was controlled by repeated exercise tolerance tests (ETT) by treadmill with the value of threshold effort time (ThT). Total duration of treatment was 4 weeks.Results. At the beginning the ThT was 249,8±23,4 s for III FC and 368,6±14,4 s for II FC patients (p=0,0001). One dose of Dlt increased ThT in 5 hours to 387,3±37,5 s and 533,7±20,3 s in both groups, respectively (p=0,001), with the difference between groups being held. During regular Dlt intake the ThT in III FC angina patients reached 441,1±26,8 s, but in II FC patients in has not changed: 526,1±22,0 s. Additional nitrate intake to III FC group led to even more increase of ThT; in II FC patients there was no improvement. Combination therapy by Dlt and nitrates has not led to differences between III and II FC groups by achieved exercise tolerance. Hemodynamic parameters in both groups has not differ.Conclusion. For patients with III FC stable angina it is recommended to prescribe Dlt with nitrates because of additional effectiveness of combination that might be linked to the influence on cardiac hemodynamics and to improvement of myocardium metabolism. In II FC stable angina Dlt alone reaches its maximum antiischemic effect so the addition of nitrates is not helpful

Adherence to Antihypertensive Therapy: A Systematic Review of Russian Prospective Studies from 2000 to 2019

Russia belongs to countries with a high prevalence of arterial hypertension (AH), which is the main cause of premature death in the Russian population. The level of blood pressure (BP) is controlled in less than a third of patients, which may be due to poor adherence to medical recommendations and irregular medication. The manuscript provides a review of studies evaluating the effectiveness of measures to improve adherence to antihypertensive therapy (AHT).Aim. To prepare a systematic review of Russian studies to assess the effectiveness of measures to increase adherence to AHT, to determine/describe the main directions of the intervention and the methodological level.Material and methods. The search for full-text articles on adherence to AHT published in Russian in the period from 2000 to 2019 was carried out in the main Russian and international electronic databases eLIBRARY.ru, Embase, Russian Medicine, MEDLINE. Of the 563 publications found, 20 were included in the review.Results. In 14 studies, adherence was assessed using the 4-item Morisky Medication Adherence Scale (MMAS-4), other studies used bespoke questionnaires or pill counts. Two studies examined factors associated with adherence. The observation period was up 6 weeks to 12 months, the number of participants is 30-2435 people. A higher adherence was noted in women, people over 50 years old, with higher education, working, with concomitant diabetes mellitus and a history of myocardial infarction. Patient education was effective interventions to improve adherence (in particular, in studies, improvement on the MMAS-4 from 1.8 to 3.9 points, p=0.0002 or from 2.80 to 3.79 points, p<0.0001), telephone reminders (p<0.0001), training in self-measurement of blood pressure (p<0.05) and fixed combinations of drugs (p<0.05).Conclusion. The most effective ways to improve adherence are patient education and the use of drugs fixed combinations. In most studies, subjective methods of adherence assessing were used