顶空固相微萃取-气相色谱/质谱法测定饮水中2-甲基异莰醇和土臭素
Detection of 2-MIB and GSM in Water by HS-SPME-GC-MS
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摘要: 目的 建立顶空固相微萃取(HS-SPME)结合气相色谱质谱联用(GC-MS)技术测定水中痕量2-甲基异莰醇(MIB)和土臭素(GSM)的方法。方法 确立检测方法的实验条件, 样品于70℃水浴经PDMS/DVB/CAR萃取30 min后, 在GC-MS上分析测定。取时间、加盐质量浓度及取样体积进行优化。结果 GC-MS测定结果显示, 在优化的实验条件下2-MIB和GSM在5~100 ng/L范围内线性关系良好, 相关系数大于0.9994, 方法的检测限分别为0.29 ng/L和0.11 ng/L; 相对标准偏差(RSD, n=6) 小于5.3%;加标回收率在93.8%~109%。结论 该方法可以用于水中痕量2-甲基异莰醇和土臭素的检测。Abstract: Objective To establish a method for the determination of 2-IBM and GSM in water by SPME/GC/MS. Methods Samples were extracted with PDMS/DVB/CAR fiber in 70℃ water bath, directly injected for GC/MS analysis, and quantified by internal standard. Results The linear range of the standard curve was in 5~100 ng/L, r>0.9994. The detection limits of 2-IBM and GSM were 0.29 ng/L and 0.11 ng/L, respectively. The RSD was below 5.3%(n=6) and the recovery was 93.8%~109%. Conclusion The method was suitable for trace analysis of 2-IBM and GSM in water.