色谱

色谱 ›› 2026, Vol. 44 ›› Issue (6): 650-657.DOI: 10.3724/SP.J.1123.2025.10015

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-串联质谱法测定生活饮用水中16种有机紫外吸收剂

王卓, 赵灿, 叶必雄*(), 陈永艳*()   

  1. 中国疾病预防控制中心环境与人群健康重点实验室，中国疾病预防控制中心环境与健康 相关产品安全所，北京 100050

Determination of 16 organic ultraviolet absorbers in drinking water by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry

WANG Zhuo, ZHAO Can, YE Bixiong*(), CHEN Yongyan*()   

  1. China CDC Key Laboratory of Environment and Population Health，National Institute of Environmental Health，Chinese Center for Disease Control and Prevention，Beijing 100050，China
  • Received:2025-10-18 Online:2026-06-08 Published:2026-06-03
  • Supported by:
    National Key Research and Development Project(2021YFC3200804)

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摘要：

有机紫外吸收剂（OUVAs）是一类近年来备受关注的新污染物。本研究针对水体中OUVAs检出率高且含量低的特点，建立了一种基于固相萃取-超高效液相色谱-串联质谱同时检测生活饮用水中9种紫外稳定剂与7种紫外过滤剂的分析方法。在500 mL水样中先加入25 mg抗坏血酸，然后加入盐酸将pH调至2~3，再加入1 mL 5 μg/L的混合内标工作液，用HLB固相萃取柱（200 mg/6 mL）对水样中的目标化合物进行富集浓缩，以Acquity Premier BEH C18（100 mm×2.1 mm，1.7 μm）色谱柱分离，甲醇-2 mmol/L乙酸铵水溶液为流动相进行梯度洗脱，采用电喷雾正离子模式电离、多反应监测模式检测，内标法定量。以饮用水作为基质，对所建立方法的精密度和准确度进行考察。结果表明，16种有机紫外吸收剂在一定范围内均呈现良好的线性关系，相关系数r均大于0.992。方法检出限（MDL，S/N=3）为0.03~5 ng/L，定量限（MQL，S/N=10）为0.1~15 ng/L。目标分析物在5、20、50 ng/L 3个加标水平下，回收率为75.0%~130.6%，相对标准偏差（RSD）为0.9%~12.9%（n=6）。用该方法对7份水源水样品和7份饮用水样品进行检测，实验结果表明，2-羟基-4-甲氧基二苯甲酮（UV-9）、奥克立林（OC）共2种有机紫外吸收剂被检出；水源水中UV-9的检出质量浓度为<MQL~13.4 ng/L，OC的检出质量浓度为5.0~32.23 ng/L。饮用水UV-9的检出质量浓度为0.4 ng/L，OC的检出质量浓度为<MQL~13.2 ng/L。该方法适用于生活饮用水中16种有机紫外吸收剂痕量分析测定，可用于我国生活饮用水中有机紫外吸收剂的环境监测分析。

关键词: 固相萃取, 超高效液相色谱-三重四极杆质谱, 有机紫外吸收剂, 饮用水

Abstract:

Organic ultraviolet absorbers （OUVAs） are a class of emerging contaminants that have garnered significant attention in recent years. In response to the characteristics of high detection frequency and low concentrations of OUVAs in water bodies， this study established an analytical method based on solid phase extraction （SPE） coupled with ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） for the simultaneous determination of 16 OUVAs （nine UV stabilizers and seven UV filters） in drinking water. The 500 mL water sample was pretreated with 25 mg ascorbic acid， acidified to pH 2-3， and spiked with 1 mL of 5 μg/L mixed internal standard working solution. Target compounds were enriched and concentrated using an HLB solid phase extraction cartridge （200 mg/6 mL）. Separation was achieved on an Acquity Premier BEH C18 column （100 mm×2.1 mm， 1.7 μm） using a gradient elution with methanol and 2 mmol/L ammonium acetate aqueous solution as the mobile phases. Detection was performed using electrospray ionization in positive mode and multiple reaction monitoring （MRM）， with quantification carried out by the internal standard method. The precision and accuracy of the established method were evaluated using drinking water as the matrix. The results showed that all 16 OUVAs exhibited good linearity within their respective mass concentration ranges， with correlation coefficients （r） greater than 0.992. The method detection limits （MDL， S/N=3） were 0.03-5 ng/L， and the method quantification limits （MQL， S/N=10） were 0.1-15 ng/L. At spiked levels of 5， 20 and 50 ng/L， the recoveries of the target analytes ranged from 75.0% to 130.6%， with relative standard deviations （RSDs） ranging from 0.9% to 12.9% （n=6）. A total of seven source water samples and seven drinking water samples were analyzed using this method. The results showed that two OUVAs， 2-hydroxy-4-methoxybenzophenone （UV-9） and octocrylene （OC） were detected. In source water， the mass concentrations of UV-9 ranged from <MQL to 13.4 ng/L， while OC mass concentrations ranged from 5.0 to 32.23 ng/L. In drinking water， UV-9 was detected at 0.4 ng/L， and OC mass concentrations ranged from <MQL to 13.2 ng/L. This method is suitable for the trace analysis of 16 OUVAs in drinking water， demonstrating good accuracy and precision. It effectively improves the detection efficiency of OUVAs in water and can be used for the environmental monitoring and analysis of OUVAs in drinking water in China.

Key words: solid phase extraction （SPE）, ultra-high performance liquid chromatography-triple quadrupole mass spectrometry （UHPLC-MS/MS）, organic ultraviolet absorbers （OUVAs）, drinking water

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