本文選題：氘 + 氨基酸��； 參考：《佳木斯大學(xué)》2014年碩士論文

【摘要】：目的尋找氘代氨基酸簡便快捷有效的合成方法，從而降低成本并根據(jù)所尋找的方法合成α-氘代氨基酸，為建立新生兒氨基酸代謝異常檢測平臺做好前期工作。 方法選擇重水交換法作為氘代氨基酸的合成方法。（1）探索反應(yīng)溫度、反應(yīng)時間和交換次數(shù)對合成氘代L-組氨酸的影響；（2）以L-[α,2,4-2H3]-組氨酸的單因素實驗條件為參考進行L-[α,2,4-2H3]-組氨酸的響應(yīng)面優(yōu)化實驗；（3）以L-[α,2,4-2H3]-組氨酸響應(yīng)面因素為參考，根據(jù)氨基酸的酸、堿、中性選擇L-[α-2H]-谷氨酸和L-[α-2H]-甲硫氨酸進行響應(yīng)面優(yōu)化實驗。（4）根據(jù)響應(yīng)面所優(yōu)化出的條件，依次合成L-[α-2H]-脯氨酸、L-[α-2H]甘氨酸、L-[α-2H]異亮氨酸以及L-[α-2H]纈氨酸。所得到氘代氨基酸經(jīng)1H-NMR測試并計算其氘代率，圓二色譜鑒定氘代后的構(gòu)型是否發(fā)生變化以及通過質(zhì)譜手段進行定性分析。 結(jié)果（1）響應(yīng)面法優(yōu)化L-[α,2,4-2H3]-組氨酸的最優(yōu)合成條件是：反應(yīng)時間為6.47h，反應(yīng)溫度為185℃，交換次數(shù)為3次。（2）響應(yīng)面法優(yōu)化L-[α-2H]-甲硫氨酸的最優(yōu)合成條件是：反應(yīng)時間6.23h，反應(yīng)溫度為182℃，，交換次數(shù)為3次。（3）響應(yīng)面法優(yōu)化L-[α-2H]-谷氨酸的最優(yōu)合成條件是：反應(yīng)時間7.15h，反應(yīng)溫度為189℃，交換次數(shù)為3次。（4）合成的氘代氨基酸經(jīng)1H-NMR鑒定氘代率均在98.5%以上，圓二色譜檢測結(jié)果表明構(gòu)型均未改變，質(zhì)譜檢測結(jié)果證明1H-NMR所得氘代數(shù)目正確。 結(jié)論重水交換法是合成氘代氨基酸的一種簡捷、高效、經(jīng)濟的實驗方法，為日后的大量生產(chǎn)提供可靠地實驗數(shù)據(jù)。并為新生兒氨基酸代謝異常檢測平臺提供的建立提供物質(zhì)基礎(chǔ)和標準圖譜。
[Abstract]:Objective to find a simple, rapid and effective method for the synthesis of deuterium amino acids, so as to reduce the cost and synthesize 偽 -deuterium amino acids according to the method, so as to establish a platform for the detection of abnormal amino acid metabolism in newborns. Methods the reaction temperature was investigated by heavy water exchange method as the synthesis method of deuterated amino acids. The effect of reaction time and exchange times on the synthesis of deuterated L-histidine.) based on the single factor experimental conditions of L- [偽-(24-2H _ 3)] -histidine, the response surface optimization experiment of L- [偽 ~ (24-2H _ 3)] -histidine was carried out using L- [偽 _ 24-2H _ 3] -histidine response surface as reference, according to the amino acid, base, amino acid, alkalinity, and the response surface of L- [偽 _ 24-2H _ 3] -histidine. Neutral selection of L- [偽 -2H] -glutamic acid and L- [偽 -2H] -methionine as response surface optimization experiment. 4) according to the optimized conditions of response surface, L- [偽 -2H] -proline L- [偽 -2H] glycine L- [偽 -2H] isocine and L- [偽 -2H] valine were synthesized in turn. The deuterium amino acids were measured by 1H-NMR and their deuterium rates were calculated. The configuration of deuterated amino acids was identified by circular dichroism and analyzed qualitatively by mass spectrometry. Results 1) the optimal conditions for the synthesis of L- [偽 -2H] -histidine by response surface method were as follows: reaction time 6.47 h, reaction temperature 185 鈩

本文編號：1925368