气相色谱-质谱联用测定长江三角洲农田土壤中的合成麝香

Determination of synthetic musks in farmland soil from Yangtze River Delta by gas chromatography-mass spectrometry

采用索氏提取、硅胶/氧化铝复合层析柱的样品前处理方法及气相色谱-质谱联用仪(GC-MS)测定长江三角洲农田土壤样品中7种合成麝香(莎利麝香、粉檀麝香、特拉斯、佳乐麝香、吐纳麝香、二甲苯麝香、酮麝香)的含量,对其污染水平和分布状况进行了研究.结果表明,实际检出的3种合成麝香(佳乐麝香、吐纳麝香、酮麝香)含量分别0.96—16.98 ng·g-1、<LOD—14.13 ng·g-1和<LOD—0.84 ng·g-1;土壤样品中合成麝香的加标回收率为88.8%—109.3%,精密度为5.8%—9.6%;仪器检出限(LOD)和定量限(LOQ)分别为0.03—0.33 ng·g-1、0.10—1.10 ng·g-1.长江三角洲农田土壤样品中普遍含有合成麝香,虽然其总浓度较低,但因其具有的生物富集性会在农产品中富集,故应做好相关的食品安全风险评价.

In this study,farmland soil samples collected from the Yangtze River Delta were extracted by Soxhlet extraction and cleaned by composite silica gel column. Seven synthetic musks（ SMs）including ADBI（ Celestolide）,AHMI（ Phantolide）,ATII（ Tonalide）,HHCB（ Galaxolide）,AHTN（ Tonalide）,MX（ Musk xylene）,MK（ Musk ketone） were analyzed by gas chromatography-mass spectrometry. The pollution level and distribution patterns of SMs were then investigated. The results indicated that the concentrations of the three SMs detected were in the range of 0. 96 to16.98 ng·g^-1,LOD to 14.13 ng·g^-1and LOD to 0. 84 ng·g^-1,respectively. The recoveries of spiked samples in soil ranged from 88.8% to 109.3%,and the relative standard deviation ranged from5.8% to 9.6%. The limit of detection and the limit of quantitation ranged from 0.03 to 0.33 ng·g^-1,0. 10 to 1. 10 ng·g^-1,respectively. SMs were ubiquitous in farmland soil samples from the Yangtze River Delta. Although the concentrations of ∑ SMs were low,they might enrich in agricultural products due to bioaccumulation. Therefore,the food safety risk evaluation is necessary.