磁性氯甲基聚苯乙烯微球固相萃取-气相色谱-串联质谱法测定环境水样中7种硝基苯类化合物

GC-MS/MS Determination of 7 Nitrobenzenes in Environmental Water Samples with Solid Phase Extraction Based on Chloromethylated Magnetic Polystyrene Nanospheres

采用磁性氯甲基聚苯乙烯微球(CMPNs)固相萃取-气相色谱-串联质谱法测定环境水样中7种硝基苯类化合物(NBs)的含量。优化的试验条件如下:(1)萃取剂为CMPNs材料;(2)CMPNs的用量为15.0mg;(3)萃取时间为4min;(4)氯化钠的加入量为340g·L^(-1);(5)洗脱剂丙酮的用量为3mL;(6)洗脱时间为1min。气相色谱分离用HP-INNOWAX色谱柱,质谱分析采用全扫描和选择离子监测模式。7种NBs的质量浓度均在0.2~4.0μg·L^(-1)内与其峰面积呈线性关系,方法的检出限(3S/N)在0.006~0.022μg·L^(-1)之间。7种NBs测定值的相对标准偏差(n=6)在0.30%~5.3%之间。方法用于环境水样的分析,回收率在72.4%~113%之间。

GC-MS/MS was applied to the determination of 7 nitrobenzenes in environmental water samples with solidphase extraction based on chloromethylated magnetic polystyrene nanospheres （CMPNs）. The optimized conditions found were as follows： （1） extracting agent.. CMPNs material; （2） amount of CMPNs： 15. 0 mg; （3） extraction time： 4 min; （4） amount of NaCl： 340 g ·L^-1; （5） amount of acetone （eluant） ： 3 mL; （6） elution time： 1 min. The HP-INNOWAX chromatographic column was used for GC separation, and the full-scanning mode and the selected ion monitoring mode were adopted in MS. Linear relationships between values of peak area and mass concentration of the 7 nitrobenzenes were kept in the same range of 0. 2- 4. 0 μg ·L^-1, with detection limits （3S/N） in the range of 0. 006-0. 022μg·L^-1. Precision of the method was tested, and values of RSD （n=6） for 7 NBs found were in the range of 0. 300//00- 5. 3%. The proposed method was applied to the analysis of environmental water samples, giving values of recovery in the range of 72. 40%-113%.