出来混迟早要还的
第11楼2009/12/13
好东西,谢谢分享. 用过MAX SPE测蓝莓效果不错,但最近测西芹却效果很差.用得是LCMSMS,不知是基质效应,还是净化部分出得问题. 不知有什么建议?
kylabs
第18楼2012/03/06
又是草甘膦啊,LCMS做草甘膦确实很难,衍生化又麻烦,提取也不容易。
以下方法供大家参考,不需要衍生化的LCMS方法,提取净化应该采用离子交换柱。
谱图在以下链接:
http://www.microsolvtech.com/hplc/app_glyphosate.asp
Method Conditions
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. |