飞行时间质谱操作规程
2.用1%甲酸溶液超声10分钟
3.用去离子水超声10分钟
4.用分析纯丙酮超声10分钟
5.用分析纯甲醇超声10分钟
6.放入盒中,自然干燥香皂包装
二,样品制备
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本实验室现有基质如下:
3-Indoleacetic acid (IAA),3-Hydroxypicolinic acid (HPA),Trihydroxyanthracene (DI),2,5-Dihydroxybenzoic acid (DHB),2',4',6'-Trihydroxyacetophenone monohydrate (THAP),2',6'-Dihydroxyacetophenone (DHAP),2-(4-Hydroxyphenylazo)benzoic acid (HABA),
根据测试人样品特点,参考相应文献报道,选择合适基质(以下表格仅供参考)
Dissolve 10 mg in 1 mL of mixed solution of acetonitrile and 0.1% TFA (2:3). Most samples such as protein, DNA, sugar, lipid and synthetic high polymer
For 1 mg of high polymer, dissolve 10 mg and 1 mg of NaCl, LiCl or KCl in demineralized water. Polar synthetic high polymer (All become Na, Li or K added ions.)
Gentisic acid, Aldrich 14,935-7 2,5-Dihydroxybenzoic acid (DHB) (C7H6O4:154.1)
Dissolve 108 mg and 16 mg of ammonium citrate dibasic in a 50% acetonitrile solution. Single stranded DNA, RNA of 50 mer or more
For 1 mg of high polymer, dissolve 10 mg in chloroform or THF. Non-polar synthetic high polymer
Dithranol, Sigma D-2773
1,8-Dihydroxy-9[10H]-anthraceno ne
(C14H10O3:226.2) For 1 mg of high polymer,
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dissolve 10 mg and 1 mg of
silver trifluoroacetate in
chloroform or THF. Non-polar synthetic high polymer (All become Ag added ions.)
Remarks:
1, 由于本仪器主要用于合成化合物的表征,故以以上两种基质使用最为广泛。
2, 基质溶液应当在每次测试前配制,如需放置隔夜,请储存于闭光、低温条件(冰箱)
三,点样
It is necessary to use methods of dropping to a sample plate that are suitable for different samples or matrices individually. This section describes the following three basic methods.
Dropping method (1): Usually used.
Dropping method (2): Used to drop a large amount of the same sample to samples. (Standard
sample in the auto analysis mode, etc.)
Dropping method (3) : Used for solid samples.
Dropping method (1)
1.Prepare an unused clean sample plate.
2.Drop 0.5μL of sample solution to the specified sample well using a pipette, etc.
Take care not allow the pipette end to touch the plate.
3.Before the crystallization of the sample (within approximately 10 seconds), drop a matrix
solution onto 0.5μL of sample solution.包覆胶水
4.Air dry.
Caution: Exchange the pipette tip every drop irrespective of matrices or sample solutions.
The dropping order of a matrix and that of a sample may be reversed mutually. Dropping method (2)
1.Prepare an unused clean sample plate.
2.Drop 20μL of matrix solution and 1.0μL of sample solution into the sample tube to mix
them.
3.Drop 1.0μL of the mixed solution to the specified sample well using a pipette, etc.
Caution: Prepare a sample solution approximately 20 times stronger than that in the dropping method (1).
Dropping method (3)
1.Prepare an unused clean sample plate.
2.Move a matrix (solid) put in a sample bottle and a sample (solid).
3.Drop an organic solvent to dissolve the matrix and the sample.
4.Drop 2.0μL of the mixed solution to the specified sample well using a pipette, etc.
四,样品分析
测定前的准备工作
打开需要的窗口
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4
三聚氰胺甲醛树脂
Acquisition window
Camera Viewer window
1 6
5
Kompact window
Spectrum Contents window
出现如上几个窗口,可以根据自己的习惯和喜好调整各窗口的位置和大小
Kompact window : 显示数据采集情况
Acquisition window : 设定仪器操作模式、设定和执行数据采集。 Spectrum Contents window :
选择要显示的采集数据
Camera Viewer window : 观察样品基激光照射位点. 设定测定参数
3
2 1
1. 选择测定模式(反射、线性、正离子、负离子)
2. 输入要测定的质量范围.
3. 激光照射频率10或5
4. 点击 Firing 标签. 设定 P .Ext: 值(与样品分子量接近)
放入样品
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2
Insert the plate as far as it will
go.
放入样品板
靶板缺角处置于右前方,其两
侧与靶板槽吻合,平行推入。
靶板槽
关闭样品门
待真空度达到 2.0E-3Pa (正离子模式)或 8.0E-4Pa (负离子模式)时可以开始采集数据.