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Rapid determination of five antipyretic analgesics in surface water by online solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry
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Ping HE1, Liqun WANG1, Shan ZHOU1, Baofeng ZHANG1, Xuan JIA1, Yi CHI1, Zhenqi XU1, Wei TANG2, *
Chinese Journal of Chromatography | 2025, 43(9) : 1063 - 1069
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Chinese Journal of Chromatography | 2025, 43(9): 1063-1069
• Articles •
Rapid determination of five antipyretic analgesics in surface water by online solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry
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Ping HE1, Liqun WANG1, Shan ZHOU1, Baofeng ZHANG1, Xuan JIA1, Yi CHI1, Zhenqi XU1, Wei TANG2, *
Affiliations
  • 1. Zhejiang Hangzhou Ecological and Environmental Monitoring Center,Hangzhou 310007,China
  • 2. Hangzhou Institute of Ecological Environment Science (Hangzhou Urban Ecological Environment Monitoring Station),Hangzhou 310014,China
Published: 2025-09-08 doi: 10.3724/SP.J.1123.2024.10018
Outline
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Antipyretic analgesics are typical pharmaceutical and personal care products (PPCPs) that are widely used in our daily life because they relieve fever and pain, and have anti-inflammatory and anti-rheumatic properties. These drugs inhibit the synthesis and release of prostaglandins (PGs) in the neurons of the anterior hypothalamus and exert therapeutic effects as a consequence. However, these drugs are relatively commonly misused and abused, often owing to a lack of proper medication guidance. As a result, these drugs enter the environment via various pathways, including wastewater treatment plants, agricultural runoff, and improper disposal, thereby posing potential threats to human health and ecosystems. The presence of these contaminants in surface water has become an environmental safety concern that necessitates the development of rapid, accurate, and high-throughput analysis methods. In this study, an analytical method was established for the determination of five antipyretic analgesics (ibuprofen, aminophenazone, antipyrine, phenacetin, and naproxen). The developed method is based on online solid phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (online SPE-UHPLC-MS/MS), which provides a high degree of automation and efficiency. Water samples were collected and filtered through 0.2-μm regenerated cellulose (RC) filter membranes, after which Na2EDTA and an internal standard were added. An aliquot (0.9 mL) of each sample was injected into the online SPE system using an automatic sampler. Samples were first adsorbed on a PLRP-S online SPE column, washed with 0.05% formic acid aqueous solution, and finally gradient-eluted with a mobile phase composed of 0.2 mmol/L ammonium fluoride solution and methanol-acetonitrile (1∶1, v/v). Analytes were separated on a ZORBAX Eclipse Plus C18 column, detected by multiple reaction monitoring with electrospray ionization in both positive- and negative-ion modes, and quantified using the internal-standard method.The five antipyretic analgesics were effectively separated under the optimized experimental conditions and showed good linearities within their respective concentration ranges, with correlation coefficients (r) greater than 0.998. The method detection limits (MDLs) ranged from 0.05 to 0.20 ng/L, and the method quantification limits (MQLs) ranged from 0.20 to 0.80 ng/L. The five antipyretic analgesics exhibited average recoveries of between 64.2% and 112%, with relative standard deviations (RSDs, n=6) of 2.06%-8.99% at low, medium, and high spiked levels. Furthermore, the method was successfully used to analyze water samples from the Hangzhou section of the Qiantang River, in which four target compounds were detected, with antipyrine found to have the highest mass concentration. This newly developed method features a high degree of automation, facilitates the injection of large volumes, and enables online enrichment, purification, and quantitative analysis in an integrated process, with minimal operational errors, high repeatability, and high sensitivity. The developed method shortens sample-analysis times, is more cost-effective, and meets the needs of large-scale sample testing, as it requires only 15 min to completely determine a sample, thereby significantly improving detection efficiency. Overall, the method features low detection limits, analyzes rapidly, and is easy to operate; hence it is suitable for rapid risk screening and the quantitative determination of antipyretic analgesics in surface water.

online solid phase extraction (online SPE)  /  ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)  /  antipyretic analgesics  /  surface water
何平, 王立群, 周姗, 张宝锋, 贾璇, 池怡, 徐珍琪, 唐伟. 在线固相萃取-超高效液相色谱-串联质谱法快速测定地表水中5种解热镇痛药物. 色谱, 2025 , 43 (9) : 1063 -1069 . DOI: 10.3724/SP.J.1123.2024.10018
Ping HE, Liqun WANG, Shan ZHOU, Baofeng ZHANG, Xuan JIA, Yi CHI, Zhenqi XU, Wei TANG. Rapid determination of five antipyretic analgesics in surface water by online solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2025 , 43 (9) : 1063 -1069 . DOI: 10.3724/SP.J.1123.2024.10018
  • National Key Research and Development Program Project(2022YFC3203403)
  • Zhejiang Ecological Environment Research and Achievement Promotion Project(2021HT0024)
  • Zhejiang Ecological Environment Research and Achievement Promotion Project(2022HT0025)
  • Zhejiang Ecological Environment Research and Achievement Promotion Project(2023HT0044)
  • Zhejiang Ecological Environment Research and Achievement Promotion Project(2022HT0003)
  • Science and Technology Development Plan of Hangzhou(20211231Y020)
Year 2025 volume 43 Issue 9
24
12
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Article Info
doi: 10.3724/SP.J.1123.2024.10018
  • Receive Date:2024-10-31
  • Online Date:2026-10-30
  • Published:2025-09-08
Article Data
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History
  • Received:2024-10-31
Funding
National Key Research and Development Program Project(2022YFC3203403)
Zhejiang Ecological Environment Research and Achievement Promotion Project(2021HT0024)
Zhejiang Ecological Environment Research and Achievement Promotion Project(2022HT0025)
Zhejiang Ecological Environment Research and Achievement Promotion Project(2023HT0044)
Zhejiang Ecological Environment Research and Achievement Promotion Project(2022HT0003)
Science and Technology Development Plan of Hangzhou(20211231Y020)
Affiliations
    1. Zhejiang Hangzhou Ecological and Environmental Monitoring Center,Hangzhou 310007,China
    2. Hangzhou Institute of Ecological Environment Science (Hangzhou Urban Ecological Environment Monitoring Station),Hangzhou 310014,China
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表12种不同金属材料的力学参数
科
Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)
属
Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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