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采用固相微萃取-气相色谱质谱法联用测定了水体中痕量多环麝香类化合物。对固相微萃取条件和解析条件进行了优化,确定了微萃取条件为:选用65μmPDMS-DVB萃取头、顶空萃取模式(HS),在800 r/min,60℃条件下,萃取45 min;萃取过程中保持pH 7并且不加入NaCl;解析条件为:解析时间为3 min,插入GC深度为4 cm,进样口温度为250℃。方法的检测限为0.29～0.37 ng/L,线性范围5～1000ng/L,相对标准偏差1.5%～2.2%。对实际污水厂不同类型的水样使用优化后的实验条件进行了验证试验,目标化合物的回收率在82.5%～92.8%之间,表明优化后的试验条件适用于实际水体中痕量多环麝香类化合物的分析测定。
Trace polycyclic musk compounds in water were determined by solid-phase microextraction-gas chromatography-mass spectrometry. The conditions of microextraction were optimized. The conditions of microextraction were determined as follows: 65 μm PDMS-DVB extraction head and headspace extraction mode (HS) were selected and extracted at 800 r / min and 60 ℃ for 45 min. During the extraction process, pH 7 was maintained and NaCl was not added. The analytical conditions were as follows: the analysis time was 3 min, the depth of GC insertion was 4 cm, and the inlet temperature was 250 ° C. The detection limits of this method ranged from 0.29 to 0.37 ng / L with a linear range of 5 ~ 1000 ng / L with relative standard deviations of 1.5% ~ 2.2%. Validation experiments were carried out on the optimized experimental conditions of different types of water samples in the actual wastewater treatment plant. The recoveries of the target compounds ranged from 82.5% to 92.8%, indicating that the optimized experimental conditions were suitable for the detection of trace polycyclic musk Analysis of compounds.