Wu Xiaogang, Chen Xiaoquan, Xiao Haijun, Liu Binqiu
Se Pu. 2015 Oct;33(10):1090-6. doi: 10.3724/sp.j.1123.2015.04045.
A method was developed for the determination of glyphosate (GLY) and glufosinate-ammonium (GLUF) in tea using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with ultrapure water and dichloromethane for 30 min under ultrasonication, followed by a simple cleanup with a C18 solid phase extraction (SPE) cartridge, and then GLY and GLUF were derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl) in borate buffer for 2 h. The derivatives of GLY and GLUF were separated on a Waters C18 column (50 mm x 2.1 mm, 1.7 μm) in a gradient elution mode, and finally detected with positive electrospray ionization-mass spectrometry (ESI-MS/MS ) in multiple reaction monitoring (MRM) mode. The quantification analysis was performed by external standard method. The method showed a good linearity (r > 0. 990) in the range of 0.003 125-0.1 mg/L. The limits of detection (LODs) of GLY and GLUF were 0.03 mg/kg. At the spiked levels of 0.375, 1.5 and 4.5 mg/kg, the recoveries of GLY and GLUF were 87.37%-99.11% and 81.44% -86.17% respectively, and the relative standard deviations (RSDs) (n = 6) of GLY and GLUF were 0.68%-1.35% and 1.01%-2.33%, respectively. This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of GLY and GLUF simultaneously in tea.
建立了一种利用超高效液相色谱 - 串联质谱法（UPLC - MS/MS）测定茶叶中草甘膦（GLY）和草铵膦（GLUF）的方法。样品用超纯水和二氯甲烷在超声条件下萃取30分钟，然后用C18固相萃取（SPE）柱进行简单净化，接着将GLY和GLUF在硼酸盐缓冲液中用9 - 芴甲氧羰基（FMOC - Cl）衍生化2小时。GLY和GLUF的衍生物在Waters C18柱（50 mm×2.1 mm，1.7μm）上以梯度洗脱模式分离，最后采用正电喷雾电离质谱（ESI - MS/MS）在多反应监测（MRM）模式下进行检测。定量分析采用外标法。该方法在0.003 125 - 0.1 mg/L范围内具有良好的线性（r＞0.990）。GLY和GLUF的检测限（LOD）为0.03 mg/kg。在加标水平为0.375、1.5和4.5 mg/kg时，GLY和GLUF的回收率分别为87.37% - 99.11%和81.44% - 86.17%，GLY和GLUF的相对标准偏差（RSD，n = 6）分别为0.68% - 1.35%和1.01% - 2.33%。该方法简单、快速，具有可接受的灵敏度和准确度，可满足同时分析茶叶中GLY和GLUF的要求。
