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Determination of 22 organophosphates and their metabolites and 11 phthalate metabolites in human whole blood by ultra performance liquid chromatography-tandem mass spectrometry
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Feiyun SHI1, Haoyu XU2, Junhong LI1, Mengyuan XU1, *
Chinese Journal of Chromatography | 2026, 44(6) : 682 - 693
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Chinese Journal of Chromatography | 2026, 44(6): 682-693
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Determination of 22 organophosphates and their metabolites and 11 phthalate metabolites in human whole blood by ultra performance liquid chromatography-tandem mass spectrometry
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Feiyun SHI1, Haoyu XU2, Junhong LI1, Mengyuan XU1, *
Affiliations
  • 1. Changzhou Center for Disease Control and Prevention,Changzhou 213022,China
  • 2. Changzhou Hospital of Traditional Chinese Medicine,Changzhou 213022,China
Published: 2026-06-08 doi: 10.3724/SP.J.1123.2025.09019
Outline
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Organic phosphate esters (OPEs) and phthalate esters (PAEs) are two classes of synthetic compounds widely incorporated into various industrial and consumer products as flame retardants and plasticizers. Both exhibit multi-organ cumulative toxicity. In this study, an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 22 OPEs and their diester metabolites (mOPEs) and 11 phthalate ester metabolites (mPAEs) in whole blood. The whole blood samples were extracted with 0.1% formic acid-acetonitrile by liquid-liquid extraction for protein precipitation, and then purified by HMR S-micro BIO 96-well solid phase extraction column. The filtrate was blown to near dryness with nitrogen, and reconstituted with 0.1% formic acid-acetonitrile solution. The target compounds were detected by UPLC-MS/MS. A Ghost Trap DS-HP chromatographic column (30 mm×2.1 mm) was used as the background ghost peak trap column, and an ACQUITY UPLC® BEH C18 chromatographic column (150 mm×2.1 mm, 1.7 μm) was used as the analytical column. Methanol and 0.5 mmol/L ammonium acetate were used as mobile phase for gradient elution. Electrospray ionization (ESI) was used for MS detection, with both positive and negative ion scanning in the multiple reaction monitoring (MRM) mode. Isotope internal standard method was used for quantification. The results showed that 33 target compounds could be separated within 15 min, and good linear relationships were observed for all target compounds across their respective mass concentration ranges (r=0.993 3-0.999 8). The limits of detection were 0.003-0.31 ng/mL and the limits of quantification were 0.01-1.02 ng/mL. The spiked recoveries of 33 targets in whole blood samples ranged from 60.5% to 138.3%, with relative standard deviations (RSDs) from 1.6% to 11.0%. The detection rates of tris-(2-chloroisopropyl)phosphate (TCiPP), triphenyl phosphate (TPHP), 2-ethylhexyl diphenyl (EHDPP), mono(2-ethyl-5-hydroxyhexyl) phthalate (MEHHP), mono-n-butyl phthalate (MNBP) and mono-n-octyl phthalate (MOP) were 100% in 14 whole blood samples, and the highest detection amount of TPHP was 10.04 ng/mL. The developed method is simple to operate, sensitive, accurate, requires small sample volumes, and is cost-effective on reagents. It is suitable for human biomonitoring, and provides a theoretical basis for monitoring organic phosphate and phthalic ester substances in the population.

organic phosphate esters  /  phthalate ester metabolites  /  whole blood  /  ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
Feiyun SHI, Haoyu XU, Junhong LI, Mengyuan XU. Determination of 22 organophosphates and their metabolites and 11 phthalate metabolites in human whole blood by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2026 , 44 (6) : 682 -693 . DOI: 10.3724/SP.J.1123.2025.09019
  • Youth Talent Science and Technology Project of Changzhou Municipal Health Commission in 2024(QN202463)
  • Youth Talent Science and Technology Project of Changzhou Municipal Health Commission in 2024(QN202425)
  • The Third Level Training Objects of the Sixth “333 High Level Talent Training Project” in Jiangsu Province [(2022) 3-4-163]
Year 2026 volume 44 Issue 6
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Article Info
doi: 10.3724/SP.J.1123.2025.09019
  • Receive Date:2025-09-28
  • Online Date:2026-07-16
  • Published:2026-06-08
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History
  • Received:2025-09-28
Funding
Youth Talent Science and Technology Project of Changzhou Municipal Health Commission in 2024(QN202463)
Youth Talent Science and Technology Project of Changzhou Municipal Health Commission in 2024(QN202425)
The Third Level Training Objects of the Sixth “333 High Level Talent Training Project” in Jiangsu Province [(2022) 3-4-163]
Affiliations
    1. Changzhou Center for Disease Control and Prevention,Changzhou 213022,China
    2. Changzhou Hospital of Traditional Chinese Medicine,Changzhou 213022,China
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https://castjournals.cast.org.cn/joweb/sepu/EN/10.3724/SP.J.1123.2025.09019
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表12种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
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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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