dd液相色谱电喷雾串联四极杆质谱法检测食物中罂粟壳残留.pdf

液相色谱- 电喷雾串联四极杆质谱法检测食物中罂粟壳残留 陈 启 廖文娟 蔡增轩 任一平 浙江省疾病预防控制中心 浙江省食品安全重点实验室 中国浙江省杭州 310009 【摘要】 本文采用液相色谱- 电喷雾串联四极杆质谱仪，用多离子反应监测 （MRM ）定量法检测 食品中的罂粟壳残留量。通过对样品SPE 净化预处理、色谱条件、质谱参数等的优化选择和方法学 验证，建立了定量检测食品中的罂粟壳残留量的理想方法。该方法对吗啡、可待因、罂粟碱、那可 丁的最低检出限LOD 分别为0.073、0.024、0.003、0.0009µg/L(进样量 10µL) ，最低定量限LOQ 分 2 别是0.24、0.08 、0.01、0.003 µg/L。在1~10 µg/L的线性范围中，相关系数r =0.999，回收率在95%~110% 以内。该方法灵敏度高、操作简单、定量准确，为食物中罂粟壳残留量检测的理想方法。 【关键字】 罂粟壳残留，三重四极杆液质联用，吗啡， 可待因， 罂粟碱， 那可丁 Determination of Pericarpium Papaveris Residues in Foods by Liquid Chromatography Tandem Mass Spectrometry Chen Qi Liao Wenjuan Cai Zengxuan Ren Yiping Zhejiang Provincial Center for Disease Prevention and Control ，Hangzhou 310009 Abstract A HPLC-MS/MS method was developed for the determination of pericarpium papaveris residues (morphine, codeine, narceine, narcotine) in foods. D -morphine was used as internal standard for 3 the quantification of pericarpium papaveris residues. For clean-up and concentration solid phase extraction (SPE) with OASIS MCX cartridges were used. LC analysis was performed on a Atlantis® MS C18 (150 ⅹ 2.0mm I.D., 5µm) column, ammonium acetate solution and methanol was used as mobile phase. The detection limits (LOD) for morphine, codeine, narceine, narcotine were 0.073, 0.024, 0.003 0.0009 µg/L respectively. The limits of quantification were 0.24, 0.08, 0.01, 0.003µg/L, respectively. The linear range was from 1 to 10µg/L with correlation coefficients of 0.999. The mean recoveries were between 95% and 110%. This method can be applied for the determination of pericarpium papaveris residues in chafing dish, contaminated oil, carbonado