06色谱联用技术要点.pptVIP

* Purity analysis of an antiulcerative drug, famotidine, shows 1 major impurity that is chromatographically resolved. Some fragmentation of the main product can help confirm the famotidine. Note that the isotope ratios in the spectra are diagnostic for the number of sulfurs present as S has a +2 isotope at about 5% abundance. A close examination of the 259 ion shows a decrease in the sulfur +2 thus confirming that the fragment lost included at least 1 sulfur. * Benzodiazepines are a class of tranquilizers which are commonly prescribed. As can be seen in this example, the benzodiazepines can be separated relatively quickly by HPLC. It should be noted that complete chromatographic resolution is not needed. Two of the peaks are highlighted and the MS spectra of these peaks will be examined next. HPLC Conditions Column: 2.1 x 100 mm HP Hypersil ODS 3 μm Flow: 400 μl/min Solvent A: 50 μM Ammonium Formate Solvent B: 10% MeOH 90% ACN Gradient: 0-1 min 30% B 1-8 min 30-75% B * Here are the mass spectra for 2 of the benzodiazepines. Note that one of the compounds, triazolam, has 2 chlorides while the other compound, diazepam, has just 1 chloride. The shift in the relationship between the pseudomolecular ion and the +2 isotope is from the chloride difference. This is a good example of the type of qualitative information that can be gleaned from the spectra. * When a pharmaceutical sample is degraded, the chromophoric region may remain intact, leading to degradation products that have similar UV-Vis spectra to the parent drug. In this example, salbutamol (aka albuterol) degadation products show this pattern of similar UV-Vis spectra. On the right, the MS TIC shows that the signal for the degraded products is very small compared to the parent drug. However, EICs for the masses detected in the degradant peaks are again very easy to quantitate and detect. * These four compounds are examples of the antibacterial class known as sulfa drugs. Show