【摘要】 针对茶叶中出现的高氯酸盐污染问题,建立液相色谱-串联质谱联用仪测定方法。样品经100 m L热水提取,于10 000 r/min下离心10 min,上清液经C18固相萃取柱净化,ZORBAX SAX色谱柱分离,以100 mmol/L乙酸铵溶液-甲醇-乙腈为流动相进行梯度洗脱,多重反应监测(MRM),外标法定量。结果表明,高氯酸盐质量浓度在0.5~200.0μg/L范围内与峰面积呈现良好线性关系,方法的加标回收率为98.9%~101.9%,相对标准偏差均<6%,检出限为0.004 mg/kg,定量限为0.01 mg/kg,具有操作简单、灵敏度高、稳定性好等优点,可很好地满足茶叶中高氯酸盐的检测和质量监管需要。更多还原

【Abstract】 For the pollution of perchlorate in tea,a method is developed for the determination of perchlorate in tea by LC-MS/MS. Perchlorate in tea are extracted with 100 m L hot water. The extract is centrifugalized at 10 000 r/min for 10 min and cleaned up on C18 solidphase extraction(SPE) column. The separation of perchlorate is carried out on a ZORBAX SAX column use 100mmol/L ammonium acetate-methanol-acetonitrile as mobile phase. The perchlorate was analyzed by LC-MS/MS under multiple reaction monitoring(MRM) and the extract was quantified by the external standard method. The results show that a good linearity is obtained for perchlorate concentration in the range of 0.5-200.0 μg/L,the recoveries of perchlorate ranged from 98.9% to101.9% with RSDs of less than 6%. The detection limit and quantitation limit of perchlorate are0.004 mg/kg and 0.01 mg/kg,respectively. The method is suitable for the determination and quality control of perchlorate in tea with a simple operation, high sensitivity, good repeatability and other significant advantages.更多还原