Analitika i Kontrol最新文献_第10页

Determination of 1-pyrenol in urine by gas chromatography with mass selective detector 气相色谱-质量选择检测器测定尿中1-芘醇

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.4.007

A. Alekseenko, O. Zhurba, A. Merinov

{"title":"Determination of 1-pyrenol in urine by gas chromatography with mass selective detector","authors":"A. Alekseenko, O. Zhurba, A. Merinov","doi":"10.15826/analitika.2019.23.4.007","DOIUrl":"https://doi.org/10.15826/analitika.2019.23.4.007","url":null,"abstract":"Urinary 1-pyrenol belongs to the biological markers of exposure to the polyaromatic hydrocarbons. Several methods for the determination of 1-pyrenol in urine necessarily include enzymatic hydrolysis, extraction from the biological sample, and derivatization with the silylating agent. Enzymatic hydrolysis and silylation take very long time: 16 hours and 40 minutes respectively. A shorter and more sensitive version of the determination of 1-pyrenol in urine by gas chromatography with mass-selective detection is proposed. Enzymatic hydrolysis with β-glucuronidase is used for 1h to digest the conjugated form of 1-pyrenol (as glucuronide). After the enzymatic hydrolysis, the analyte is extracted from the biological matrix by hexane extraction, followed by evaporation of the extract to dry residue in an inert gas stream. The optimum conditions for liquid extraction are established by varying the ratio of salting out agent : extraction time : extraction ratio. The dry residue is re-dissolved and derivatized in the silylating reagent N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) into trimethylsilyl ether at room temperature for 5 minutes. The analysis of the trimethylsilyl extract is carried out by gas chromatography on HP-5MS capillary column with mass-selective detection. The analyte is identified by the retention time and the ratio of the main and confirming ions. The high-accuracy determination is ensured by using the internal standard 1-pyrenol-d 9 . The range of detectable concentrations of the method is from 0.1 to 100 μg/l. Repeatability and interlaboratory precision are 4.4% and 6.4% respectively. The systematic error turns out to be insignificant. The accuracy is 14%. The method is tested on the urine samples of workers with the main professions in the aluminum production industry.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67251855","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Application of a molecularly imprinted polymer based on the polyimide as a piezosensor selective coating for determining the oleic acid in oils 基于聚酰亚胺的分子印迹聚合物作为一种压电传感器选择性涂层用于测定油中的油酸

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.1.006

C. N. Linh, О. V. Duvanova, A. N. Zyablov

{"title":"Application of a molecularly imprinted polymer based on the polyimide as a piezosensor selective coating for determining the oleic acid in oils","authors":"C. N. Linh, О. V. Duvanova, A. N. Zyablov","doi":"10.15826/analitika.2019.23.1.006","DOIUrl":"https://doi.org/10.15826/analitika.2019.23.1.006","url":null,"abstract":"При создании селективных пьезоэлектрических сенсоров на основе полимеров с молекулярными отпечатками (ПМО) рассмотрена возможность применения квантово-химического моделирования для выбора условий их синтеза. Исходным полимером для получения ПМО являлась полиамидокислота (ПАК), представляющая собой сополимер 1,2,4,5-бензолтетракарбоновой кислоты с 4,4′-диаминодифенилоксидом. При двухступенчатой термоимидизации раствора ПАК в присутствии темплата образовывался полиимид с молекулярным отпечатком. В качестве темплата служила олеиновая кислота. Оптимизацию структур и вычисление энергий проводили с использованием программы Gaussian 09 гибридным методом функционала плотности B3LYP в базисе 6-31G(d,p) с коррекцией ошибки суперпозиции базисных наборов BSSE (basis set superposition error). Показано, что структура радикала жирной кислоты играет решающую роль в образовании отпечатков и, соответственно, в селективности полимера. На основании проведенных квантово-химических расчетов установлено оптимальное соотношение реагентов в предполимеризационной смеси 4 : 1. Методом нековалентного импринтинга синтезированы полимеры с молекулярными отпечатками олеиновой кислоты на поверхности пьезоэлектрических сенсоров. Экспериментально оценена способность полученных сенсоров к распознаванию этой кислоты в модельных бинарных и тройных смесях жирных кислот, установлено, что сенсор на основе полимера с молекулярными отпечатками наиболее чувствителен к олеиновой кислоте, предел обнаружения которой составил 0.14 г/дм3. Пьезоэлектрические сенсоры на основе ПМО апробированы при определении жирной кислоты в растительных маслах (подсолнечное, кукурузное, оливковое, льняное, рапсовое), в качестве метода сравнения использовали хромато-масс-спектрометрию и установили, что разность результатов определения менее 10 %. Ключевые слова: полимеры с молекулярными отпечатками, полиамидокислота, полиимид, олеиновая кислота, компьютерное моделирование, модифицированные пьезосенсоры.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67249106","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 2

Improving the organic solvents purity for microextraction preconcentration of impurities 提高有机溶剂纯度，用于杂质的微萃取预富集

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.1.008

V. Krylov, P. V. Mosygin, L. Smirnov, S. A. Bulanova, I. A. Zhituhina, G. V. Pushkarev

引用次数: 0

Effect of modifier nature on the preconcentration efficiency of rutin and quercetin on the magnetite nanoparticles 改性剂性质对芦丁、槲皮素在磁铁矿纳米颗粒上富集效率的影响

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.2.012

I. S. Reshetnikova, S. S. Aleksenko, S. Shtykov

引用次数: 0

Analytical control of food systems on the acrylamide content using the method of highly efficient liquid chromatography with mass-spectrometric detection 高效液相色谱-质谱法检测食品体系中丙烯酰胺含量的分析控制

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.3.002

A. V. Kulikovskii, N. Vostrikova, O. Kuznetsova, A. Semenova, A. Ivankin

引用次数: 1

Sample injection of aromatic compounds from passive concentrators into multicapillary column by the thermal desorption method 用热解吸法将被动浓缩器中的芳香族化合物样品注入多毛细管柱

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.3.003

V. M. Gruznov, M. Baldin, A. Malysheva

引用次数: 0

Determination of trace elements in plants using the direct current arc atomic-emission spectrometry 用直流电弧原子发射光谱法测定植物中微量元素

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.3.011

I. E. Vasil’eva, E. Shabanova

{"title":"Determination of trace elements in plants using the direct current arc atomic-emission spectrometry","authors":"I. E. Vasil’eva, E. Shabanova","doi":"10.15826/analitika.2019.23.3.011","DOIUrl":"https://doi.org/10.15826/analitika.2019.23.3.011","url":null,"abstract":"Plants connect together the atmosphere, the biosphere and the hydrosphere, participate in the migration of chemical elements and indicate an anthropogenic environmental pollution. For this reason, it is important to determine the content of a wide range of essential and toxic elements in plants. Atomic emission spectrometry with different sources of excitation of atoms is one of the most frequently used instrumental methods for determining the elemental composition of plants. Express determination of 23 essential and toxic elements in plant powders (without ashing and acid decomposition) using the atomic emission spectrometry with arc discharge (DC-arc AES) was developed. The special ways of obtaining spectra and of spectral information processing provided an increased accuracy of the analytical results in the concentration ranges from n ∙(10 -6 -10 -4 ) to 10 wt. %. The trueness of the results of the developed technique was verified by the means of the encrypted certified reference materials of the plants and matching them with the results obtained by the certified techniques of atomic emission and mass spectrometry with inductively coupled plasma. The application of the DC-arc AES technique to determine trace elements in plants from the ecologically clean and polluted areas with different landscapes, provided new analytical data for the interdisciplinary research. These data are traceable to the well-known international certified reference materials of plants.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67251829","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 2

Determination of Catharanthus flower anthocyanins 花楸花花色苷的测定

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.1.001

V. I. Deinek, Y. Kulchenko, А. N. Sidorov, S. M. Varushkina, I. Blinova, L. А. Deineka, A. Vu

引用次数: 1

Extraction-fluorimetric determination of chlorophyll "a" in the natural waters 提取-荧光法测定天然水体中叶绿素a

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.3.001

Z. Temerdashev, L. Pavlenko, Y. S. Ermakova, I. Korpakova, B. D. Eletskii

引用次数: 1

Poly-4-vinylpiridinium nanosponges as modifiers of the electrophoretic systems for the charged analytes separation 聚-4-乙烯基吡啶纳米海绵作为带电分析物分离电泳系统的改性剂

Analitika i Kontrol Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.3.006

D. Polikarpova, D. Makeeva, L. Kartsova, V. Davankov, L. Pavlova

{"title":"Poly-4-vinylpiridinium nanosponges as modifiers of the electrophoretic systems for the charged analytes separation","authors":"D. Polikarpova, D. Makeeva, L. Kartsova, V. Davankov, L. Pavlova","doi":"10.15826/analitika.2019.23.3.006","DOIUrl":"https://doi.org/10.15826/analitika.2019.23.3.006","url":null,"abstract":"Novel hydrophilic ionic polymer nanoparticles based on the N-alkylated hypercrosslinked poly-4-vinylpyridine (nanosponges ‒ NS ) have porous structure, pH-independent positive charge and contain the aromatic rings. These nanosponges have not yet been studied in the capillary electrophoresis mode, but their characteristics suggest the possibility of creating the fused silica capillary walls coating for the separation of anionic and cationic analytes. In the current research, the authors, for the first time, have proposed the approaches to the formation of coatings based on the nanosponges with a molecular weight of 400 and 10 kDa. It was established that the stability of such coatings could be achieved by the introduction of NS into the background electrolyte. The pH range of background electrolytes for the subsequent electrophoretic experiments was determined to be from 4 to 9. The NS-based coatings were compared with the previously investigated coatings based on the crosslinked polystyrene nanoparticles ( NPs ), functionalized with the quaternary ammonium groups. Capillaries modified with NS (400 kDa) were tested for the electrophoretic separations of wide range of analytes: carboxylic acids, aminoacids, fluoroquinoline antibiotics, biogenic amines, and proteins. The separation selectivity of carboxylic acids on the NS-modified capillaries was different from the separation selectivity on the capillaries modified with NPs, functionalized with quaternary ammonium groups. NS affect the separation selectivity of aminoacids by interacting with these analytes, while for fluoroquinoline antibiotics NS act as an agent generating the reversed electroosmotic flow ( EOF ). The modification of fused silica capillary walls by NS with molecular mass of 400 kDa prevented the sorption of biogeniс amines and lysozyme protein during their electrophoretic separation.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67250516","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0