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雾非雾
第4楼2013/07/19
Gas Liquid Chromatographic Determination of 4 Chlorophenoxyacetic Acid Residues in Mung Bean Sprouts
Gas-liquid chromatographic determination of 4-chlorophenoxyacetic acid residues in mung bean sprouts.
J Assoc Off Anal Chem 1982 Sep;65(5):1118-21
Wong YS.
A gas-liquid chromatographic (GLC) method is described for determining 4-chlorophenoxyacetic acid (CPA) residues in mung bean sprouts. The residues were extracted from samples by using ethyl acetate followed by liquid-liquid partition into 5% NaHCO3 solution. After acidification and reextraction with ethyl acetate, CPA was reacted with pentafluorobenzyl bromide (PFB-Br) to form the PFB derivative. The reaction mixture was separated on a silica gel column to remove excess reagent, and the derivative was eluted with a solution of 75% toluene in hexane. GLC separations were performed on a 3% OV-1 column at 230 degrees C. As low as 10 pg CPA could be quantitated, which is equivalent to about 0.05 ppm at residue level, using an electron capture detector. Recoveries of CPA from fortified mung bean sprouts (0.05, 0.20, and 0.50 ppm) ranged from 71 to 107%. The PFB derivative was further identified by gas chromatography-mass spectrometry.
雾非雾
第6楼2013/07/19
色谱柱:Kinetex™ 2.6 µm PFP 100 Å, $$lc Column 50 x 2.1 mm, Ea
尺寸:50 x 2.1 mm ID
洗脱类型:Isocratic
洗脱A:0.1% Formic acid in Water
洗脱B:0.1% Formic acid in Acetonitrile
梯度:
步骤顺序 | 时间 (分) | 流动相A | 流动相B |
1 | 4 | 70 | 30 |
流速:0.8 mL/min
冷却温度:25 °C
检测:UV-Vis Abs.-Variable Wave.(UV) @ 280 nm (25°C)
备注:SecurityGuard™ ULTRA Guard Cartridge System extends column lifetime.
- SecurityGuard ULTRA Cartridges, UHP$$lc PFP for 2.1mm ID Columns, 3/Pk Part No.: AJ0-8787
- Holder Part No.: AJ0-9000
色谱柱:Luna® 3 µm PFP(2) 100 Å, $$lc Column 150 x 4.6 mm, Ea
尺寸:150 x 4.6 mm ID
洗脱类型:Gradient
洗脱A:0.1% Formic acid in Water
洗脱B:0.1% Formic acid in Acetonitrile
梯度:
步骤顺序 | 时间 (分) | 流动相A | 流动相B |
1 | 0 | 45 | 55 |
2 | 6 | 25 | 75 |
流速:1 mL/min
冷却温度:室温
检测:UV-Vis Abs.-Variable Wave.(UV) @ 280 nm (22°C)
备注:SecurityGuard™ Guard Cartridge System extends column lifetime.
- SecurityGuard Cartridges, PFP 4 x 3.0 mm, 10/Pk Part No.: AJ0-8327
- Holder Part No.: KJ0-4282