kylabs
第2楼2011/04/07
给你一个LCMS的谱图和条件:
Column | Cogent Diamond Hydride™, 4µm, 100A |
Catalog No. | 70000-15P-2 |
Dimensions | 2.1 x 150 mm |
Solvents | A: DI water + 5 mM ammonium acetate B: 90% acetonitrile/10% DI water/10 mM ammonium acetate |
Gradient | 0.0 min ?80.0%B 1 .0 min 80%B 1.1 min to 5%B 5.0 min 5%B 6.0 min to 80%B |
Post time | 5 min |
Flow rate | 0.5 mL/min. |
Sample Prep | Glyphosate: 168.0067m/z (M - H)- Figure A: injection #1, RT = 3.365 min Figure B: injection #5, RT = 3.366 min Sample stock solution was purchased from Sigma (1000 mcg/mL). Sample for analysis was made by diluting the stock 1:100 in 30:70 solution A and B. |
Detection | ESI ?neg - Agilent 6210 MSD TOF mass spectrometer. |
庸人
第4楼2011/04/08
感谢你提供的资料!
我用的是正离子模式,其实从草胺磷的性质来说,是一个偏酸性的化合物,从常理说可能要选择负离子模式,但根据一些文献(也包括外文的),用正离子的较多,所以就必须要求最后的制备液pH值应较低才行。这里我不知道到底是负离子模式下不稳定还是什么原因,因这是给别人代做的,自己做的前期工作少,也没深入的去查相关的资料!⊙﹏⊙b汗。。。。
改天有时间我用负离子重新做一下,再一次感谢你提供的资料!
Column | Cogent Diamond Hydride™, 4µm, 100A |
Catalog No. | 70000-15P-2 |
Dimensions | 2.1 x 150 mm |
Solvents | A: DI water + 5 mM ammonium acetate B: 90% acetonitrile/10% DI water/10 mM ammonium acetate |
Gradient | 0.0 min ?80.0%B 1 .0 min 80%B 1.1 min to 5%B 5.0 min 5%B 6.0 min to 80%B |
Post time | 5 min |
Flow rate | 0.5 mL/min. |
Sample Prep | Glyphosate: 168.0067m/z (M - H)- Figure A: injection #1, RT = 3.365 min Figure B: injection #5, RT = 3.366 min Sample stock solution was purchased from Sigma (1000 mcg/mL). Sample for analysis was made by diluting the stock 1:100 in 30:70 solution A and B. |
Detection | ESI ?neg - Agilent 6210 MSD TOF mass spectrometer. |