分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
9期
1235-1239
,共5页
介孔材料%有机小分子%基质辅助激光解析飞行时间质谱
介孔材料%有機小分子%基質輔助激光解析飛行時間質譜
개공재료%유궤소분자%기질보조격광해석비행시간질보
Mesoporous Silica%Small organic molecules%Matrix-assisted laser desorption/ionization-time of flight-mass spectrometry
研究了表面修饰的无机有机复合型介孔材料SBA-15-NA(1,8-Naphthalimide)作为基质在MALDI-TOF-MS分析中的应用。采用1,8-萘酰亚胺修饰SBA-15,1,8-萘二甲酸酐先与3-三甲氧基硅基-1-丙胺反应,得到的产物再修饰到SBA-15,得到SBA-15-NA,应用修饰后的介孔材料SBA-15-NA为基质获得了具有背景离子干扰少、离子化效率高、更高的峰值强度等优点的谱图。甲醇作为溶剂,分析物和基质的浓度比例为1∶10,采用以样品和基质等体积混合均匀点样方法,对低糖类、氨基酸类、植物激素生物代谢物和药物等不同结构的小分子化合物(分子量小于500)进行了 MALDI-TOF-MS 分析。在此优化的条件下得到了低检出限1×10-9 g/L(亮氨酸,信噪比为5)和高重现性(≤30%)。采用衍生化的复合型介孔材料直接测定了实际尿样。
研究瞭錶麵脩飾的無機有機複閤型介孔材料SBA-15-NA(1,8-Naphthalimide)作為基質在MALDI-TOF-MS分析中的應用。採用1,8-萘酰亞胺脩飾SBA-15,1,8-萘二甲痠酐先與3-三甲氧基硅基-1-丙胺反應,得到的產物再脩飾到SBA-15,得到SBA-15-NA,應用脩飾後的介孔材料SBA-15-NA為基質穫得瞭具有揹景離子榦擾少、離子化效率高、更高的峰值彊度等優點的譜圖。甲醇作為溶劑,分析物和基質的濃度比例為1∶10,採用以樣品和基質等體積混閤均勻點樣方法,對低糖類、氨基痠類、植物激素生物代謝物和藥物等不同結構的小分子化閤物(分子量小于500)進行瞭 MALDI-TOF-MS 分析。在此優化的條件下得到瞭低檢齣限1×10-9 g/L(亮氨痠,信譟比為5)和高重現性(≤30%)。採用衍生化的複閤型介孔材料直接測定瞭實際尿樣。
연구료표면수식적무궤유궤복합형개공재료SBA-15-NA(1,8-Naphthalimide)작위기질재MALDI-TOF-MS분석중적응용。채용1,8-내선아알수식SBA-15,1,8-내이갑산항선여3-삼갑양기규기-1-병알반응,득도적산물재수식도SBA-15,득도SBA-15-NA,응용수식후적개공재료SBA-15-NA위기질획득료구유배경리자간우소、리자화효솔고、경고적봉치강도등우점적보도。갑순작위용제,분석물화기질적농도비례위1∶10,채용이양품화기질등체적혼합균균점양방법,대저당류、안기산류、식물격소생물대사물화약물등불동결구적소분자화합물(분자량소우500)진행료 MALDI-TOF-MS 분석。재차우화적조건하득도료저검출한1×10-9 g/L(량안산,신조비위5)화고중현성(≤30%)。채용연생화적복합형개공재료직접측정료실제뇨양。
Mesoporous silica SBA-15 with a small organic molecular (1,8-Naphthalimide) was synthesized and used as matrix for MALDI-TOF-MS ( Matrix-assisted laser desorption/ionization time of flight mass spectrometry) analysis. A modified SBA-15 matrix, SBA-15-NA (1,8-Naphthalimide) was synthesized by covalently attaching SBA-15 to an 1 , 8-naphthalimide formed by 1 , 8-naphthalic anhydride and 3-( trimethoxysilyl) propylamine. The mass spectra obtained with SBA-15-NA exhibited less background interference ions, higher desorption/ionization efficiency, and higher peak intensity. The matrix was initially prepared in methanol and mixed with analyte at a 1∶1 volume ratio in vial. The solution of mixture was at a 10∶1 concentration ratio of matrix/analyte on a stainless steel target and allowed to air dry. The method was used to analyze various types of low molecular weight ( less than 500 ) chemical compounds such as monosaccharides, amino acids, phytohormones, drugs. Under the optimal conditions, it gave low detection limit of 1×10-9 g/L (Leucine, S/N=5) and good reproducibility (≤30%). The modified mesoporous silica materials have been employed in the urinary study for direct detection of metabolites.