Citation: SUN Yi-Lin, KANG Yang, ZHENG Long-Fang, ZHANG Wan-Ru, MA Ai-Xin, ZHAO Jian, WANG Xiao, ZHAO Xian-En. Determination of Endocrine Disruptors by High Performance Liquid Chromatography-Fluorescence Detection Using Magnetic Dispersive Solid Phase Extraction[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(1): 86-92. doi: 10.19756/j.issn.0253-3820.181534 shu

Determination of Endocrine Disruptors by High Performance Liquid Chromatography-Fluorescence Detection Using Magnetic Dispersive Solid Phase Extraction

1.
Shandong Provincial Key Laboratory of Life-organic Analysis, Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu 273165, China;
2.
Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology(Shandong Academy of Sciences), Jinan 250014, China

Received Date: 16 August 2018
Revised Date: 10 October 2018

Fund Project: This work was supported by the National Natural Science Foundation of China (Nos. 21775088, 81303179).

A new high performance liquid chromatography-fluorescence detection (HPLC-FLD) method was developed by fluorescence derivatization and magnetic dispersive solid phase extraction (MDSPE) technology for the determination of triclosan (TCS), β-estradiol (E2), nonylphenol (NP), and 4-octylphenol (OP). With 2'-carbonyl chloride rosamine (RHB-Cl) as precolumn derivatization reagent, the derivatization and MDSPE conditions were investigated. The results showed that the maximum derivatives were obtained after derivatizationin for 5 min in Na₂CO₃-NaHCO₃ buffer solution at pH 9.5 at room temperature (20℃). Under the optimized conditions including using magnetic graphene oxide as MDSPE adsorbent (15 mg), extraction for 5 min, methanol/acetic acid (9:1, V/V) as elution agent, and elution for 3 min, four endocrine disruptor compound derivatives were enriched and purified. Under optimized chromatographic conditions, the four derivatives were separated within 12 min. The fluorescence excitation and emission wavelengths were set at 554 nm and 570 nm, respectively, achieving highest detection sensitivity for four endocrine disruptor compounds derivatives. The limits of detection (LODs) were in the range of 1.1-1.9 ng/L, and the limits of quantification (LOQs) were in the range of 4.0-7.5 ng/L. This method had good linearity, precision and recovery results, and also showed obvious advantages such as simplicity, rapidity and high sensitivity comparing to the reported methods. It was a convenient and validated method for the routine analysis of endocrine disruptor compounds in milk, toothpaste and waste water, and could provide a new method for food, drinking and water safety supervision.
- Magnetic graphene oxide,
- Dispersive solid phase extraction,
- Derivatization,
- High performance liquid chromatography,
- Endocrine disruptor compounds,
- Milk,
- Environmental water
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沈阳化工大学材料科学与工程学院沈阳 110142