搅拌棒萃取-气相色谱-质谱法分析地表水中合成麝香及紫外线吸收剂

Determination of Synthetic Musks and UV Filters in Surface Water by Stir Bar Sorption Extraction and Gas Chromatography-Mass Spectrometry

  • 摘要: 建立了搅拌棒萃取-溶剂解吸结合气相色谱-质谱法测定水样中16种合成麝香及2种紫外线吸收剂。实验优化了萃取温度、萃取时间、萃取体积、pH值、离子强度、溶剂解吸条件等参数,最终确定使用50 mL水样在40 ℃下搅拌提取4 h后,采用1.2 mL溶剂超声解吸后直接浓缩分析。该方法的线性范围为2~120 μg/L,线性相关系数大于0.996,各化合物的加标回收率在68.5%~126%之间,相对标准偏差范围为2.3%~14.9%,方法检出限在0.003~0.038 μg/L之间。应用该方法分析北京市内不同采样点的7个地表水样品,结果表明,佳乐麝香的检出率最高,浓度在0.003~0.337 μg/L之间。该方法操作简单、有机溶剂使用量少,可以实现分析测试快速、绿色的目的,能够用于实际水样中合成麝香和紫外线吸收剂的同时准确分析。

     

    Abstract: A method for simultaneous determination of 16 synthetic musks (including 5 nitro musks, 6 polycyclic musks and 5 macrocyclic musks) and 2 UV filters (BP-3 and UV-P) in water samples was developed by stir bar sorption extraction (SBSE) with liquid desorption (LD), coupled with gas chromatography-mass spectrometry (GC/MS). In order to get good extraction efficiencies of the target compounds, the important factors affecting the stir bar sorption extraction procedure were discussed, such as extraction time, temperature, stirring speed, volume of sample, pH value, ionic strength, content of organic modifier, different extraction solvents for desorption and the time of liquid desorption by ultrasound extraction. Finally, 50 mL water sample with certain amount of surrogate was stirred extraction for 4 h at 40 ℃ with magnetic stir bar of PDMS, the stirring speed was 950 r/min. Then the stir bar was resolved twice with acetonitrile-acetone solvent. The extract was concentrated to 0.5 mL and added the internal standard for injection. The chromatographic separation was carried on a DB-5MS Ultra Inert column (30 m×0.25 mm×0.25 μm) and detected by mass spectrometry at selected ion monitoring (SIM) mode. The results show that 16 synthetic musks and 2 UV filters have good linearity, the linear range of this method is 2-120 μg/L, while the correlation coefficients (R2) are more than 0.996. The recoveries of three spiked level range from 68.5% to 126%, the relative standard deviations (RSDs) of this method are 2.3%-14.9%, and the limits of detection (LOD) range from 3 μg/L to 0.038 μg/L. Moreover, the method was applied to detect surface water samples in Beijing. The results show that the detection rate of HHCB is the highest, and the concentration is between 0.003 μg/L and 0.337 μg/L. In conclusion, this method is suitable for the rapid analysis of 16 synthetic musks and 2 UV filters in water samples with easy operation, less organic solvent consumption, and can be applied to the accurate analysis of synthetic musks and UV filters in actual surface water samples.

     

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