水中呋喃丹及草甘膦的检测除了柱后衍生还有别的方法吗

xiaokeke870614

2012/01/30

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液相色谱（LC）

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该帖子已被版主-蓝人加2积分，加2经验;加分理由:鼓励深入研究

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kylabs

第1楼2012/01/30

草甘膦有一个非衍生的方法：
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.

Discussion

A reliable method for the determination of glyphosate is presented. Analysis was performed using a Cogent Diamond Hydride™ HPLC column which provides very reproducible retention and fast equilibration even when a gradient analysis is used. The use of LC-MS detection allows avoiding time consuming derivatization of this compound which is lacking a chromophore for UV detection. The method shown, with ANP retention avoids derivatization, which is required when an ordinary C18 column is used.

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tangtang

第2楼2012/01/30

Cogent Diamond Hydride这根柱子是不是比较特殊？

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kylabs

第3楼2012/01/30

属于特殊的亲水柱，通常可以运行反反相（水系正相，ANP）模式对亲水化合产生保留。
tangtang(tangtang) 发表:Cogent Diamond Hydride这根柱子是不是比较特殊？

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xiaokeke870614

第4楼2012/02/02

请问这个方法是出自哪儿的呢？

kylabs(kylabs) 发表:草甘膦有一个非衍生的方法：
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.