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Development of a HPLC-MS/MS method for determination of L-dopa in human blood serum
Neumannová, Johana ; Kozlík, Petr (advisor) ; Křížek, Tomáš (referee)
The diploma thesis is focused on the development of a high-performance liquid chromatography in conjunction with tandem mass spectrometry detection (HPLC-MS/MS) for the determination of L-dopa in human blood serum. Levodopa is a dopamine precursor and is generally used to treat Parkinson's syndrome. The tandem mass spectrometry detection and the high-performance liquid chromatography method were optimized. The optimal conditions were as follows: HALO 90 Å Penta-HILIC column (150 x 2,1 mm; 2,7 µm), Advanced Materials Technology (USA). The mobile phase used was a mixture composed of 0,1% formic acid (component A) and acetonitrile (component B) under gradient elution. The total analysis time was 12,50 minutes, the flow rate was 0,4 ml min-1, a 5 µl sample was injected, the autosampler temperature was 15 řC and the column temperature was 40 řC. The following MRM transitions in positive mode were monitored: 1. levodopa: m/z 198,1 → m/z 152,1 (Q1: -10 V, CE: -16 V, Q3: -28 V) 2. deuterated levodopa (IS): m/z 201,1 → m/z 155,2 (Q1: -10 V, CE: -14 V, Q3: -28 V) The setting of the ion source was as follows: the nebulization gas flow 3 l min-1, the drying gas flow 10 l min-1, the internal temperature 300 řC, the capillary voltage 3 000 V, the desolvation capillary temperature 250 řC. In the end of the work,...
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Using levoglucosenone in the synthesis of naphthoquinone containing compounds
Neumannová, Johana ; Matoušová, Eliška (advisor) ; Baszczyňski, Ondřej (referee)
This bachelor thesis is focused on using levoglucosenone in the synthesis of the naphthoquinone containing compounds. Levoglucosenone is a versatile and easily available substance which can be prepared by pyrolysis of renewable cellulose-containing materials. The synthesis of the target compound begins with the preparation of the substrate for the tandem reaction (propargyl ether) in three steps. The following key steps of the synthesis include palladium-catalyzed tandem cyclization/Suzuki cross coupling and subsequent Heck reaction. Oxidation of the prepared methoxy-substituted naphthalene yields the o-naphthoquinone, which has a similar structure as some naturally occurring substances with naphthoquinone skeleton, e.g. mansonone D and populene C. Key words: Synthesis, naphthalenes, naphthoquinones, levoglucosenone, catalysis, polycyclic compounds
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