DETERMINATION OF RISPERIDONE IN BIOLOGICAL MATERIAL BY ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY
ВИЗНАЧЕННЯ РИСПЕРИДОНУ В БІОЛОГІЧНОМУ МАТЕРІАЛІ МЕТОДОМ УЛЬТРАЕФЕКТИВНОЇ РІДИННОЇ ХРОМАТОГРАФІЇ
| dc.creator | Trush, H. S. | |
| dc.creator | Halkevych, I. Y. | |
| dc.date | 2016-10-28 | |
| dc.date.accessioned | 2020-02-26T12:37:45Z | |
| dc.date.available | 2020-02-26T12:37:45Z | |
| dc.identifier | https://ojs.tdmu.edu.ua/index.php/pharm-chas/article/view/6828 | |
| dc.identifier | 10.11603/2312-0967.2016.3.6828 | |
| dc.identifier.uri | https://repository.tdmu.edu.ua/handle/123456789/15008 | |
| dc.description | Introduction. Risperidone is an antipsychotic medication from neuroleptic group. It used to treat schizophrenia, psychotic depression, manic symptoms and autism. On chemical structure it is derivative of benzisoxazole – 3-[2-[4-(6-fluoro-1, 2-benzisoxazol-3-yl)-1-piperidinyl] ethyl]-6, 7, 8, 9-tetrahydro-2-methyl-4H-pyrido- [1, 2-a]-pyrimidin-4-one . It is a selective monoaminergic antagonist with high affinity to 5HT 2-serotoninergic and D 2 dopaminergic receptors.Aim of investigation is an elaboration of condition of quantitative and qualitative determination of risperidone using UPLC/MS/MS in internal organs.Materials and methods. Risperidone standard was received from Sigma-Aldrich (USA). Methanol was HPLC grade (Merck). Acetonitrile and formic acid was received from Merck (Darmstadt,Germany). Water was purified by Milli-Q Ultrapure Water System (Waters) and used for preparing of formic acid solution. 96 % ethanol, 25 % ammonium solution, and oxalic acid were analytical grade.Condition of LC-ESI-MS/MS determination. Risperidone analysis was performed on Acquity H-class UPLC system (Waters,Milford,USA) equipped with BEH C18 (2.1×50 mm, 1.7 μm) column (Waters,Milford,USA). Linear gradient elution was applied for analysis. Gradient consisted of 0.1 % formic acid in water (solvent A) and acetonitrile (solvent B). Flow rate was set to 0.5 ml/min, initial conditions were 100 % A for 1 min, followed by 40 % A for 1.5 min and 100 % A for 1 min. MS/MS data was obtained with Xevo TQD triple quadrupole mass spectrometer detector (Waters Milford, USA). Analysis was performed in positive electrospray ionization mode. Capillary voltage was set to 2 kV, source temperature –120°C, desolvation temperature –400°C, desolvation gas flow – 800 l/h, cone gas flow – 25 l/h. MRM transition for risperidone was monitored at 411 > 191.Standart solution. Risperidone stock solutions were prepared in methanol (1.0 mg/ml). Working standards were prepared from the stock solution with the final concentrations of 0.5; 1.0; 5,0; 10.0; 20.0; 50.0; 100.0; 500.0 and 1000/0 ng/ml.Preparing of biological sample. Risperidone was isolated from brain and liver tissues with water acidified by oxalic acid; and the extracts were purified on GraceResolv™ Silica 5g/25ml columns. An eluent was 0.5 % ammonia solution in ethanol. Samples of biological material were investigated after 6 or 24 hours of preparing.Results and discussion. Risperidone identified in the chromatogram for the retention time (tR = 2,91 ± 0,07 min) and the presence of signals at 411>119 m/z. Within risperidone concentrations of 0.5 to 20 ng / ml calibration plot is Y = 4.98 ·104X-1.32·104 (correlation coefficient r = 0.9998); and the concentration range of 20 to 1000 ng/ml this dependence is Y = 5.07·104X - 1,28·104 (r = 0.99995); where Y – area of the peak, X – risperidone concentration (ng /ml).The GraceResolv columns allow to isolate 76.90% - 82.27% risperidone from acidic exstracts of liver and 75.3% - 81.08% – from brain. The results of a series of parallel studies are reproducible.Conclusions. UPLH/MS/MS method on BEN C18 column with MRM monitoring m/z at 411> 191 has been developed for risperidone determination in biological tissues.GraceResolv ™ Silica columns isolates 76,9-82,3% of risperidone from liver extracts and 75.3-81.1% – from brain.LOD of risperidone for liver tissue is 1 ng/g, for brain tissue is 1.4 ng/g; LOQ of this compound is 1.6 ng / g and 2 ng / g respectively. | en-US |
| dc.description | Запропоновано умови ідентифікації та кількісного визначення рисперидону методом ультраефективної рідинної хроматографії з тандемною мас-спектрометрією на колонці BEH C18 в зразках біологічного матеріалу. Витяжки отримували шляхом настоювання гомогенізованих проб печінки та мозку з водою, підкисленою оксалатною кислотою. Кислі витяжки очищали методом флеш-хроматографії на колонках GraceResoIv ™ SiIica 5g / 25mI (Grace, USA). Як елюент використано 0,5 % розчин аміаку в 96 % етанолі. | uk-UA |
| dc.format | application/pdf | |
| dc.language | ukr | |
| dc.publisher | Тернопільський державний медичний університет імені І. Я. Горбачевського МОЗ України | uk-UA |
| dc.relation | https://ojs.tdmu.edu.ua/index.php/pharm-chas/article/view/6828/6232 | |
| dc.rights | Авторське право (c) 2016 Фармацевтичний часопис | uk-UA |
| dc.rights | https://creativecommons.org/licenses/by-nc-nd/4.0 | uk-UA |
| dc.source | Pharmaceutical Review; No. 3 (2016); 22-25 | en-US |
| dc.source | Фармацевтичний часопис; № 3 (2016); 22-25 | uk-UA |
| dc.source | 2414-9926 | |
| dc.source | 2312-0967 | |
| dc.source | 10.11603/2312-0967.2016.3 | |
| dc.subject | risperidone | en-US |
| dc.subject | brain | en-US |
| dc.subject | liver | en-US |
| dc.subject | flash chromatography | en-US |
| dc.subject | ultra high liquid chromatography (UPLC-MS/MS) | en-US |
| dc.subject | рисперидон | uk-UA |
| dc.subject | мозок | uk-UA |
| dc.subject | печінка | uk-UA |
| dc.subject | флеш-хроматографія | uk-UA |
| dc.subject | ультраефективна рідинна хроматографія (УЕРХ/МС/МС) | uk-UA |
| dc.title | DETERMINATION OF RISPERIDONE IN BIOLOGICAL MATERIAL BY ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY | en-US |
| dc.title | ВИЗНАЧЕННЯ РИСПЕРИДОНУ В БІОЛОГІЧНОМУ МАТЕРІАЛІ МЕТОДОМ УЛЬТРАЕФЕКТИВНОЇ РІДИННОЇ ХРОМАТОГРАФІЇ | uk-UA |
| dc.type | info:eu-repo/semantics/article | |
| dc.type | info:eu-repo/semantics/publishedVersion |
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