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LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY (HPLS-MS-MS) AS METHOD FOR SEPARATION AND IDENTIFICATION OF NEW ANTI-INFLAMMATORY AGENT FROM DERIVATIVES OF THIADIAZOLILAMIDE
DOI: https://doi.org/10.29296/25877313-2018-04-03
Issue:
4
Year:
2018
Objective. Development of the HPLC-MS / MS technique for the separation and identification of new anti-inflammatory drugs from the thiadiazolamide group. Material and methods. Non-steroid anti-inflammatory drugs from the group of thiadiazolylamide derivatives – acexazolamide, pyridazolamide and nitrobenzolamide were the objects of this study. Chromatography was performed using an Agilent 1260 Infinity II chromatograph (Agilent InfinityLab Poroshell 120 analytical columns EC-C18 2.7 μm 4.6 × 100 mm, Agilent Zorbax Eclipse Plus C18 5 μm 4.6 × 150 mm). As a mobile phase, a mixtures of acetonitrile, methanol, deionized water and formic acid was used in different ratios in isocratic or gradient modes. Identification of new anti-inflammatory agents from the thiadiazolamide group was carried out mass-spectrometrically using a triple quadrupole mass spectrometer AB Sciex QTrap 3200 MD with an electrospray ion source (Turbo V with a TurboIonSpray probe). Results. a high performance liquid chromatography technique with tandem mass spectrometry (HPLC-MS / MS) was developed to separate and identify new anti-inflammatory agents from the thiadiazolamide group (Zorbax Eclipse Plus C18 analytical column 5 μm 4.6 × 150 mm, gradient elution: 1-2 , 5 min 30% acetonitrile, 0.6 ml/min 2.5 - 12 min 70% acetonitrile, 1.2 ml/min, analysis time 3 minutes, mass spectrometric detection). The retention time of acexazolamide, pyridazolamide and nitrobenzolamide was 2.05, 2.22 and 2.70 minutes respectively. The identification of thiadiazolylamides was carried out by mass spectrometry. Detection conditions: negative polarization, electrospray voltage - 5500.0 V, decasterization potential of acexazolamide, pyridazolamide and nitrobenzenamide -170,0; -140.5, -280.0 V at a curtain gas pressure of 20.0 psi and a spray gas of 40.0 psi, a rate of 10 μl/min. The input potential for all ions was -4.5 V, the scan range was 200-300 Da. The values of MRM transitions with negative polarization were for azexazolamide m/z 282.8 → 73.1 m/z 282.8 → 128 and m /z 282.8 → 196.1; for nitrobenzenamide m/z 276.9 → 189.9, m/z 276.9 → 144.2 and m/z 276.9 → 122.1; for pyridazolamide m/z 232.9 → 146.2, m/z 232.9 → 78.0 and m/z 232.9 → 102.9. Conclusion. The developed HPLC-MS / MS technique allows the detection of new non-steroid anti-inflammatory drugs from the group of thiadiazolamide derivatives in one sample without their separation
Keywords:
HPLS-MS/MS
chromatography
mass-spectrometry
thiadiazolilamides
non-steroid anti-inflammatory drug
References:
- Kazaishvili Ju.G., Malygin A.S., Popov N.S. Issledovanie protivoallergicheskoj, anal'geticheskoj i protivovospalitel'noj aktivnosti novyh proizvodnyh tiadiazola // Materialy Mezhdunar. nauchno-praktich. konf.«Nauka i obrazovanie v XXI veke» (30 sentjabrja 2013,Tambov). 2013. T. 1. S. 81−83.
- Kazaishvili Ju.G., Demidova M.A. Issledovanie anal'geticheskoj aktivnosti novyh proizvodnyh tiadiazola // Sovremennye problemy nauki i obrazovanija. 2012. № 6. URL: www.science-education.ru/106-7306.
- Popov N.S., Demidova M.A. Otsenka ostroj toksichnosti novogo aminokislotnogo proizvodnogo tiadiazola pri vnutribrjushinnom vvedenii mysham // Verhnevolzhskij meditsinskij zhurnal. 2016. T. 15. Vyp. 1. S. 9–12.
- Popov N.S., Demidova M.A. Otsenka ul'tserogennosti novogo aminokislotnogo proizvodnogo tiadiazola privnutrizheludochnom vvedenii krysam // Vrach-aspirant.2017. № 1(80). S. 71–78.
- Arpit K., Basavaraj M., Sarala P., Sujeet K.,Satyaprakash K.Synthesis and pharmacological activity of imidazo[2,1 b][1,3,4]thiadiazole derivatives // Acta Poloniae Pharmaceutica, Drug Research. 2016. V. 73. № 4. P. 937–947.