超高效液相色谱-三重四极杆质谱法测定地表水和废水中8种紫外线吸收剂OA
Determination of eight ultraviolet absorbers in surface water and wastewater by ultra performance liquid chromatography-triple quadrupole mass spectrometry
紫外线吸收剂是一种广泛应用于工业的光稳定剂,具有高持久性和生物蓄积性,难以通过自然方式降解,可能长期残留在环境中,并通过食物链累积,对生态系统和生物多样性造成不可逆的损害.本研究建立了一种基于液液萃取-超高效液相色谱-三重四极杆质谱测定地表水和废水中 8 种紫外线吸收剂的方法.量取 100 mL水样,采用二氯甲烷液液萃取,氮吹浓缩,甲醇复溶,加入内标混匀后,通过 BEH C18 色谱柱(100 mm×2.1 mm,1.7 μm)分离,以 0.2%甲酸水溶液-乙腈为流动相进行梯度洗脱,多反应监测(MRM)模式检测,内标法定量.8 种紫外线吸收剂在 1~100 ng/mL范围内线性良好,方法检出限为 1.3~2.8 ng/L,方法定量限为 5.2~11.2 ng/L,在低、中、高 3 个加标水平下的回收率为 80.3%~117.8%,相对标准偏差为 1.4%~10.5%.将该方法应用于 10 份印染废水样品的检测,废水中共检出 UV-329、UV-326、UV-328、UV-350 这 4 种紫外线吸收剂,其中 UV-329 检出率最高,且检出的质量浓度占比高达 85%,检出质量浓度范围为 5.2~2 109 ng/L.该方法灵敏度好,准确度高,可应用于地表水和废水中紫外线吸收剂的检测.
Ultraviolet(UV)absorbers are a group of chemicals widely used in various industrial and consumer products,such as plastics,coatings,and personal care products,to protect against UV radiation.Among them,benzotriazole derivatives(e.g.UV-326,UV-327,UV-328,UV-329,and UV-P)are the most frequently employed.Owing to their widespread use and potential persistence in the environment,these compounds have been detected in various environmental matrices,including surface water,wastewater,sediment,and biota.Certain UV stabilizers have been reported to exhibit endocrine-disrupting properties and pose potential ecological risks.Therefore,developing sensitive and reliable analytical methods for monitoring these compounds in environmental samples is essential.To address the need for reliable detection methods,this study developed a robust method based on liquid-liquid extraction(LLE)coupled with ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)for the simultaneous de-termination of eight UV absorbers in surface water and wastewater.Critical optimization of the pretreatment process focused on solvent selection and purification parameters.The finalized protocol involved extracting 100 mL water samples twice with dichloromethane.After nitrogen-assisted solvent evaporation,the residue was reconstituted in methanol and mixed with the internal standard so-lution.UPLC-MS/MS parameters were optimized to achieve optimal instrumental performance.The separation of the eight UVs was performed using a BEH C18 column(100 mm×2.1 mm,1.7 μm)with a gradient elution system consisting of 0.2%(mass fraction)formic acid aqueous solution and acetonitrile at a flow rate of 0.4 mL/min.The injection volume was 2 μL.Detection was performed in positive ion mode using multiple reaction monitoring(MRM),with an electrospray ionization voltage set at 5 500 V.Quantification was achieved via internal standard calibration to ensure precision and accuracy.The method demonstrated excellent linearity for all target compounds across their respective concentration ranges,with a correlation coefficient(r)>0.995.The method detection limits(MDLs)ranged from 1.3 ng/L to 2.8 ng/L,indicating high sensitivity.Recovery tests conducted at low,medium,and high spiking levels(20,200,and 800 ng/L)yielded recoveries of 80.3%-117.8%,with relative standard deviations(RSDs)of 1.4%-10.5%,confirming the method's robustness across different sample matrices.Application of the method to 10 textile dyeing wastewater samples revealed the presence of four UV absorbers:UV-329,UV-326,UV-328,and UV-350.Notably,UV-329 showed the highest detection frequency and accounted for 85%of the total detected mass concentrations,ranging from 5.2 to 2 109 ng/L.Its prevalence suggests its widespread use in industrial processes and potential persistence in aquatic environments.In conclusion,the developed method is highly sensitive,accurate,and reliable for detecting UV absorbers in environmental water samples.Its successful application to surface water and wastewater analysis provides a valuable tool for monitoring these emerging contaminants,thereby supporting the assessment of their environmental and health risks.This study highlights the importance of continued monitoring and regulation of UV absorbers to mitigate their potential adverse effects on ecosystems and human health.
孙慧婧;张蓓蓓;黄梦乔;王荟;胡冠九;陈慧敏
江苏省环境监测中心,国家环境保护地表水环境有机污染物监测分析重点实验室,江苏 南京 210019江苏省环境监测中心,国家环境保护地表水环境有机污染物监测分析重点实验室,江苏 南京 210019江苏省淮安环境监测中心,江苏 淮安 223001江苏省环境监测中心,国家环境保护地表水环境有机污染物监测分析重点实验室,江苏 南京 210019江苏省环境监测中心,国家环境保护地表水环境有机污染物监测分析重点实验室,江苏 南京 210019上海爱博才思分析仪器贸易有限公司,上海 200335
化学化工
紫外线吸收剂超高效液相色谱-三重四极杆质谱液液萃取
ultraviolet(UV)absorbersultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)liquid-liquid extraction(LLE)
《色谱》 2026 (4)
413-421,9
江苏省生态环境监测科研基金项目(24B01)国家自然科学基金面上项目(22376098). Jiangsu Provincial Ecological Environment Monitoring Scientific Research Fund Project(No.24B01)the National Natural Science Foundation of China(No.22376098).
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