VALIDATION METHOD FOR DETERMINATION OF THE SULFUR HEXAFLUORIDE IN PLASMA SAMPLES OF EXPERIMENTAL ANIMALS
A new GCMS-based method for quantitative determination of active substance of new contrast drug based on sulfur hexafluoride (SH) in the rat blood plasma is produced. A ratio plot of peak area of sulfur hexafluoride to peak area of internal standard toluene [y, S(SH)/S(toluene)] versus concentration...
| Main Authors: | , , , , , |
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| Format: | Article |
| Language: | Russian |
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LLC Center of Pharmaceutical Analytics (LLC «CPHA»)
2019-01-01
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| Series: | Разработка и регистрация лекарственных средств |
| Subjects: | |
| Online Access: | https://www.pharmjournal.ru/jour/article/view/171 |
| _version_ | 1826569804320866304 |
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| author | S. S. Vlasov S. V. Krivoshchekov M. K. Zamanova M. V. Belousov A. M. Guriev M. S. Yusubov |
| author_facet | S. S. Vlasov S. V. Krivoshchekov M. K. Zamanova M. V. Belousov A. M. Guriev M. S. Yusubov |
| author_sort | S. S. Vlasov |
| collection | DOAJ |
| description | A new GCMS-based method for quantitative determination of active substance of new contrast drug based on sulfur hexafluoride (SH) in the rat blood plasma is produced. A ratio plot of peak area of sulfur hexafluoride to peak area of internal standard toluene [y, S(SH)/S(toluene)] versus concentration of sulfur hexafluoride (x, µL/mL) was linear over 0.003-0.500 µL/mL. The calibration graph can be described by the equation y=0.9526x+0.0037 (r2=0.9990). Limit of quantitation (LOQ) (signal-to-noise 10,12) was 0.003 µL/mL. Inter- and intra-serial accuracy related to nominal concentrations were 100.40-101.20% and 86.67-110.0%, respectively. The RSD values for inter- and intra-serial accuracy were 3.68-4.15% and 1.23-10.68%, respectively. The samples of the same series with SH concentrations 0.01 µL/mL and 0.50 µL/mL were analyzed in order to determine the stability. Samples were stored for 24 hours to determine the short-term stability. To determine the long-term stability Samples were stored for 25 days. Short-term stability at room temperature were 0.52% and 1.86% and long-term stability at -20 °C were -90.43% and -81.81% for SH concentrations 0.01 µL/mL and 0.50 µl/ml, respectively. Accuracy during freezing and thawing of samples were 102.30% and 100.10% and RSD values were 5.40% and 1.50%, respectively. |
| first_indexed | 2024-04-10T01:41:22Z |
| format | Article |
| id | doaj.art-6646330ff02045c1a5a28536d09b3a33 |
| institution | Directory Open Access Journal |
| issn | 2305-2066 2658-5049 |
| language | Russian |
| last_indexed | 2025-03-14T11:45:09Z |
| publishDate | 2019-01-01 |
| publisher | LLC Center of Pharmaceutical Analytics (LLC «CPHA») |
| record_format | Article |
| series | Разработка и регистрация лекарственных средств |
| spelling | doaj.art-6646330ff02045c1a5a28536d09b3a332025-03-02T09:53:18ZrusLLC Center of Pharmaceutical Analytics (LLC «CPHA»)Разработка и регистрация лекарственных средств2305-20662658-50492019-01-0104174179171VALIDATION METHOD FOR DETERMINATION OF THE SULFUR HEXAFLUORIDE IN PLASMA SAMPLES OF EXPERIMENTAL ANIMALSS. S. Vlasov0S. V. Krivoshchekov1M. K. Zamanova2M. V. Belousov3A. M. Guriev4M. S. Yusubov5National Research Tomsk Polytechnic UniversityNational Research Tomsk Polytechnic UniversityNational Research Tomsk Polytechnic UniversitySiberian State Medical UniversitySiberian State Medical UniversityNational Research Tomsk Polytechnic UniversityA new GCMS-based method for quantitative determination of active substance of new contrast drug based on sulfur hexafluoride (SH) in the rat blood plasma is produced. A ratio plot of peak area of sulfur hexafluoride to peak area of internal standard toluene [y, S(SH)/S(toluene)] versus concentration of sulfur hexafluoride (x, µL/mL) was linear over 0.003-0.500 µL/mL. The calibration graph can be described by the equation y=0.9526x+0.0037 (r2=0.9990). Limit of quantitation (LOQ) (signal-to-noise 10,12) was 0.003 µL/mL. Inter- and intra-serial accuracy related to nominal concentrations were 100.40-101.20% and 86.67-110.0%, respectively. The RSD values for inter- and intra-serial accuracy were 3.68-4.15% and 1.23-10.68%, respectively. The samples of the same series with SH concentrations 0.01 µL/mL and 0.50 µL/mL were analyzed in order to determine the stability. Samples were stored for 24 hours to determine the short-term stability. To determine the long-term stability Samples were stored for 25 days. Short-term stability at room temperature were 0.52% and 1.86% and long-term stability at -20 °C were -90.43% and -81.81% for SH concentrations 0.01 µL/mL and 0.50 µl/ml, respectively. Accuracy during freezing and thawing of samples were 102.30% and 100.10% and RSD values were 5.40% and 1.50%, respectively.https://www.pharmjournal.ru/jour/article/view/171gas chromatography-tandem mass spectrometrysulfur hexafluorideultrasound contrast agents |
| spellingShingle | S. S. Vlasov S. V. Krivoshchekov M. K. Zamanova M. V. Belousov A. M. Guriev M. S. Yusubov VALIDATION METHOD FOR DETERMINATION OF THE SULFUR HEXAFLUORIDE IN PLASMA SAMPLES OF EXPERIMENTAL ANIMALS Разработка и регистрация лекарственных средств gas chromatography-tandem mass spectrometry sulfur hexafluoride ultrasound contrast agents |
| title | VALIDATION METHOD FOR DETERMINATION OF THE SULFUR HEXAFLUORIDE IN PLASMA SAMPLES OF EXPERIMENTAL ANIMALS |
| title_full | VALIDATION METHOD FOR DETERMINATION OF THE SULFUR HEXAFLUORIDE IN PLASMA SAMPLES OF EXPERIMENTAL ANIMALS |
| title_fullStr | VALIDATION METHOD FOR DETERMINATION OF THE SULFUR HEXAFLUORIDE IN PLASMA SAMPLES OF EXPERIMENTAL ANIMALS |
| title_full_unstemmed | VALIDATION METHOD FOR DETERMINATION OF THE SULFUR HEXAFLUORIDE IN PLASMA SAMPLES OF EXPERIMENTAL ANIMALS |
| title_short | VALIDATION METHOD FOR DETERMINATION OF THE SULFUR HEXAFLUORIDE IN PLASMA SAMPLES OF EXPERIMENTAL ANIMALS |
| title_sort | validation method for determination of the sulfur hexafluoride in plasma samples of experimental animals |
| topic | gas chromatography-tandem mass spectrometry sulfur hexafluoride ultrasound contrast agents |
| url | https://www.pharmjournal.ru/jour/article/view/171 |
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