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    聚酰胺固相萃取结合高效液相色谱-串联质谱法测定广东省水源水中8种双酚类化合物的含量

    Determination of 8 Bisphenol Compounds in Source Water in Guangdong Province by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Polyamide Solid Phase Extraction

    • 摘要: 提出了聚酰胺固相萃取结合高效液相色谱-串联质谱法(HPLC-MS/MS)测定广东省水源水中双酚A、双酚AP、双酚B、双酚AF、双酚F、双酚E、双酚Z和双酚C等8种双酚类化合物的含量。取500 mL水样过填装1.00 g聚酰胺的固相萃取柱,用6 mL甲醇洗脱,取1 mL洗脱液过0.22 µm尼龙针式过滤器,采用HPLC-MS/MS测定其中8种双酚类化合物的含量,以Acquity UPLC BEH C18色谱柱为固定相,以不同体积比的0.1 mmol·L-1碳酸氢铵溶液-甲醇混合液为流动相进行梯度洗脱,基质匹配法定量。结果表明,双酚类化合物的质量浓度在一定范围内与对应的峰面积呈线性关系,检出限(3S/N)为0.12~10.50 ng·L-1。按照标准加入法进行回收试验,回收率为73.3%~111%,测定值的相对标准偏差(n=5)为1.4%~12%。方法用于从广东省11个城市采集的14份自来水、11份江河水、3份山泉水、2份水库水、2份湖水和1份井水样品的分析,结果显示8种双酚化合物的检出率为3.03%~87.88%,平均质量浓度为0.18~290.22 ng·L-1,平均质量浓度总和为327.48 ng·L-1

       

      Abstract: A method for determination of 8 bisphenol compounds, including bisphenol A, bisphenol AP, bisphenol B, bisphenol AF, bisphenol F, bisphenol E, bisphenol Z, and bisphenol C, in source water from Guangdong Province was proposed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) with polyamide solid phase extraction. The water sample (500 mL) was passed through a solid phase extraction column packed with 1.00 g of polyamide, followed by elution with 6 mL of methanol. The eluent (1 mL) was filtered through a 0.22 µm-nylon needle filter, and the 8 bisphenol compounds were determined by HPLC-MS/MS using Acquity UPLC BEH C18 column as the stationary phase and a mixed solution composed of 0.1 mmol·L−1 ammonium bicarbonate aqueous solution and methanol at different volume ratios as the mobile phase for gradient elution, with quantitative analysis by matrix matching method. As shown by the results, linear relationships between the corresponding peak areas and mass concentrations of the bisphenol compounds were kept in definite ranges, with detection limits (3S/N) in the range of 0.12-10.50 ng·L−1. Test for recovery was made by the standard addition method, giving results in the range of 73.3%-111%, and RSDs (n=5) of the determined values ranged from 1.4% to 12%. This method was applied to the analysis of 14 tap water samples, 11 river water samples, 3 spring water samples, 2 reservoir water samples, 2 lake water samples, and 1 well water sample collected from 11 cities in Guangdong Province. It was shown that the detection rates of the 8 bisphenol compounds ranged from 3.03% to 87.88%, with average mass concentrations in the range of 0.18-290.22 ng·L−1 and the total average mass concentration of 327.48 ng · L−1.

       

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