摘要
建立了气相色谱-质谱法测定茶叶中噻嗪酮残留量的方法。茶叶中残留的噻嗪酮用丙酮-正己烷混合溶剂(1∶1)提取,提取液经Envi-Carb活性碳柱和LC-Alumina N中性氧化铝柱净化,浓缩定容后,直接用气相色谱-质谱进行分析和确证,外标法定量。以HP-5MS(30m×0.25mm i. d., 0.25 μm)石英毛细管柱为分离柱,噻嗪酮的分离效果良好。方法的线性范围为0.01～1.00μg/mL,检出限为0.01mg/kg,回收率为81.6％～97.2％,相对标准偏差为3.36％～5.78％。质谱监测离子选m/z为105、140、172、305amu,其强度比约为41∶13∶29∶17。样品前处理采用微量化学技术。
The method for the determination of the residual buprofezin in teas by gas chromatography - mass spectrometry was established. The residual buprofezin in teas was extracted by acetone - hexane (1:1) , the extract was cleaned by active carbon column and neutral alumina column. After concentrated to a definite volume, it was analyzed and identified by GC-MS, quantified by external standards. A good separation was obtained using HP - 5MS(30 m ×0. 25 mm i. d. ,0. 25μm) capillary quartz column. The linear range of this method was 0.01 - 1.00 μg/mL, detection limit was 0.01mg/kg for tea samples, the recovery was 81. 6% -97.2% and the RSD was 3. 36% - 5. 78% . The m/z 105 , 140, 172, 305 amu were chosen as mass spectrometry monitoring ions, the intensity radios were about 41:13:29:17 respectively. The sample extraction was performed according to the microchemical method.
出处
《化学分析计量》
CAS
2002年第1期7-9,共3页
Chemical Analysis And Meterage
