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Simultaneous determination of caffeine, ergotamine, and metamizol in solid pharmaceutical formulation by HPTLC-UV-FLD with mass confirmation by online HPTLC-ESI-MS.
| Content Provider | Semantic Scholar |
|---|---|
| Author | Aranda, Mario Morlock, Gertrud E. |
| Copyright Year | 2007 |
| Abstract | A new high-throughput method is developed to quantify caffeine, ergotamine, and metamizol in a solid pharmaceutical formulation. After dissolution, the compounds are separated on silica gel 60 F(254) high-performance thin-layer chromatography (HPTLC) plates with ethyl acetate-methanol-ammonia 90:15:1 (v/v/v) as the mobile phase. Detection is performed by UV absorption at 274 nm for caffeine and metamizol, and by fluorescence at 313 /> 340 nm for ergotamine. Calibrations are linear or polynomial with determination coefficients (R(2)) >or= 0.9986. Recoveries of the three compounds are between 95% and 102% at three different concentration levels. Repeatability [relative standard deviation (RSD)] of all substances in the matrix is between +/- 0.9% and +/- 1.7%. Intermediate precision (RSD) of the three compounds range from +/- 2.0% to +/- 3.1%. Mass confirmation is performed by a single quadrupole mass spectrometry in positive electrospray ionization full scan mode for caffeine and ergotamine and in negative mode for metamizol. The results proved that this method is a simple and reliable alternative for routine analysis. |
| Starting Page | 1 |
| Ending Page | 5 |
| Page Count | 5 |
| File Format | PDF HTM / HTML |
| Alternate Webpage(s) | https://oup.silverchair-cdn.com/oup/backfile/Content_public/Journal/chromsci/45/5/10.1093/chromsci/45.5.251/2/45-5-251.pdf?Expires=1493026586&Key-Pair-Id=APKAIUCZBIA4LVPAVW3Q&Signature=PxZQzq8zgdXKu39-1vicHa3jWOy6klCizzt~vga0Z~qLzqc0m4LEo4eR72MjfPcohyZLYAs7zbBkEHaynjGIxHwYUrJ0De5pW2C~JAR4GCjU1kU0dBAfhBSn6DMcNWw8DDP-7PTkfkEyrgM4S3-wZ3MV-0OAqu~L55RqLMVpGlBivJscbrEJwaa4v2AdISH1-C5ShYrco3QQwNqne8E-ofkm1~FwoFB8n-dIo37kk49YjDX54m~0uWnOSc5EyizVou~x49yDqni7LA1nlTcQR1ySSl0ylHvkrf6XwoAVknaALyV~Q0485HOm8bbEKnUFs0W6uZmzJDGiRphCCtafIQ__ |
| PubMed reference number | 17555632v1 |
| Volume Number | 45 |
| Issue Number | 5 |
| Journal | Journal of chromatographic science |
| Language | English |
| Access Restriction | Open |
| Subject Keyword | Ammonia Caffeine Calibration Dipyrone Dosage Forms Eluent Ergotamine Fluorescence Methanol Physiological Sexual Disorders Quadrupole Recovery - action Silica Gel Silicon Dioxide Spectrometry Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization Standard deviation Thin Layer Chromatography Tracer Volume fraction confirmation - ResponseLevel ethyl acetate |
| Content Type | Text |
| Resource Type | Article |
