固相萃取-气相色谱-质谱法同时检测饮用水中的18种农药残留

发布时间：2018-03-11 13:08

  本文选题：农药　切入点：水　出处：《中国卫生检验杂志》2016年03期 　论文类型：期刊论文

【摘要】：目的建立水中18种农药的固相萃取-气相色谱-质谱分析方法。方法利用C_(18)固相萃取小柱预处理水样,通过对固相萃取条件的优化,得出了最佳实验条件:水样加0.5 g氯化钠和2 ml甲醇作为改进剂,上样流速为10 ml/min,洗脱溶剂为乙酸乙酯和正己烷,洗脱体积为10 ml,洗脱速率为2 ml/min;GC-MS采用HP-5MS石英毛细管色谱柱(30 m×0.25 mm,0.25μm)分离18种农药,氦气为载气,柱流量为1.0 ml/min,进样体积为1.0μl。选择电子轰击离子源(EI),辅助线温度为280℃,离子源温度为230℃,四极杆温度为150℃;加入菲-d10作为内标,利用选择离子监测(SIM)模式进行定性定量。结果 18种农药的方法检出限为0.000 07 mg/L~0.000 31 mg/L,加标回收率为72.5%~105.1%,相对标准偏差(RSD)为1.1%~9.7%。结论本法同时测定水中18种农药,操作简便、省时、灵敏,环境污染小。
[Abstract]:Objective to establish a solid phase extraction (SPE)-gas chromatography-mass spectrometry (SPC-MS) method for the determination of 18 pesticides in water. The optimum experimental conditions were obtained as follows: the water sample was modified with 0.5 g sodium chloride and 2 ml methanol, the flow rate of the sample was 10 ml / min, the elution solvent was ethyl acetate and n-hexane, The elution volume was 10 ml and the elution rate was 2 ml 路min ~ (-1) GC-MS. 18 pesticides were separated by HP-5MS quartz capillary column (30 m 脳 0.25 mm ~ (25) 渭 m). Helium gas was used as carrier gas, column flow rate was 1.0 ml / min, and sample volume was 1.0 渭 L. the electron bombardment ion source was selected and the auxiliary line temperature was 280 鈩，

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