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本研究建立了固相萃取(SPE)-超高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF-MS)检测沉积物中水杨酸(SA)、萘普生(NAX)、布洛芬(IBU)、酮洛芬(KET)、双氯芬酸(DIC)、降固醇酸(CLO)和三氯生(TRI)7种新型污染物的分析方法。样品用甲酸-丙酮溶液(1∶99,V/V)超声提取,MAX阴离子固相萃取柱净化,UPLC-QTOF-MS测定。在优化的实验条件下,7种新型污染物在2~500μg/L浓度范围内线性关系良好,线性相关系数均大于0.99,方法检出限(S/N=3)为0.5~0.6μg/kg,方法定量限(S/N=10)为1.5~2.0μg/kg(均以干重计),3个添加浓度水平(低、中、高)的回收率为87.8%~105.1%,相对标准偏差(n=5)为3.1%~12.2%。利用该方法对广州市流溪河段表层沉积物样品进行分析,检出4种污染物,最高浓度范围为6.51~12.26μg/kg(以干重计)。该方法高效、准确,适用于沉积物中7种污染物的测定。
In this study, UPLC-QTOF-MS was developed for the determination of salicylic acid (SA), naproxen (NAX) and buluolide in sediments by solid phase extraction (SPE) (IBU), Ketofen, Diclofenac, CLO and TRI. The samples were extracted with formic acid-acetone solution (1:99, V / V), purified with MAX anion-exchange chromatography and analyzed by UPLC-QTOF-MS. Under the optimized experimental conditions, the linearity of the seven new pollutants was good in the concentration range of 2 ~ 500μg / L with the linear correlation coefficients greater than 0.99. The detection limit (S / N = 3) was 0.5 ~ 0.6μg / kg (S / N = 10) was 1.5 ~ 2.0μg / kg (all based on dry weight). The recoveries of three concentrations (low, medium and high) were 87.8% -105.1% Deviations (n = 5) ranged from 3.1% to 12.2%. The samples of surface sediment in Liuxi section of Guangzhou City were analyzed by this method. Four kinds of pollutants were detected, the highest concentration range was 6.51 ~ 12.26μg / kg (dry weight basis). The method is efficient and accurate and suitable for the determination of seven pollutants in sediments.