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MICROCHEMICAL JOURNAL · 2020 · IF 3.594

Supramolecular imprinted polymeric stir bar sorptive extraction followed by high-performance liquid chromatography for endocrine disruptor compounds analysis

Zhimin Liu,Zhigang Xu,Yujian Liu,Yuanchen Liu,Baohua Lu,Liping Ma

Molecular imprinted coatings based on β -cyclodextrin ( β -CD) and acrylamide functional monomers were presented. The supramolecularly imprinted polymeric (SMIP) adsorption materials employed as the coatings of stir bar sorptive extraction (SBSE) for endocrine disruptor compounds (EDCs) analysis were proposed. A series of derivatized β -CDs functional monomers were synthesized and characterized. The best couple of functional monomers used for SMIP was selected from the β -CD monomers and common functional monomers, respectively. The ratio of two functional monomers was also optimized. The SMIP coatings showed good selectivity to the bisphenol A template and its structural analogs. It also provided enrichment factors ranging from 56 to 160 for bisphenols, which were 32- to 1600-fold higher than that of the commercial polyacrylate fibers (85 μm, Supelco). Moreover, the SMIP coatings displayed better selectivity and extraction amount than the nonimprinted and both single-functional monomer-based imprinted coatings, respectively. Therefore, the SMIP coatings triggered off a synergetic recognition for target analytes. The developed SMIP-SBSE-HPLC method was successfully applied for three environmental estrogen analysis in real water samples. A recovery of 92–119% and relative standard deviation of 1.6–9.7% were obtained. Taken together, the supramolecular imprinting strategy can provide new ideas for the development of novel supramolecular polymer-based adsorption materials, and can provide an efficient analytical method for the selective analysis of trace substances in environmental water samples.

研究领域: 分析化学 · 环境科学 · 材料科学
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JOURNAL OF CHROMATOGRAPHY A · 2013 · IF 4.612

Polydimethylsiloxane/metal-organic frameworks coated stir bar sorptive extraction coupled to high performance liquid chromatography-ultraviolet detector for the determination of estrogens in environmental water samples

Cong Hu,Man He,Beibei Chen,Cheng Zhong,Bin Hu

In this work, three kinds of metal-organic frameworks (MOFs), MOF-5, MOF-199 and IRMOF-3, were introduced in stir bar sorptive extraction (SBSE) and novel polydimethylsiloxane (PDMS)/MOFs (including PDMS/MOF-5, PDMS/MOF-199 and PDMS/IRMOF-3) coated stir bars were prepared by sol–gel technique. These PDMS/MOFs coatings were characterized and critically compared for the extraction of seven target estrogens (17-β-estradiol, dienestrol, diethylstilbestrol, estrone, 4-t-octylphenol, bisphenol-A and 17α-ethynylestradiol) by SBSE, and the results showed that PDMS/IRMOF-3 exhibited highest extraction efficiency. Based on the above facts, a novel method of PDMS/IRMOF-3 coating SBSE-high performance liquid chromatography ultraviolet (HPLC-UV) detection was developed for the determination of seven target estrogens in environmental waters. Several parameters affecting extraction of seven target estrogens by SBSE (PDMS/IRMOF-3) including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N   =   3) were found to be in the range of 0.15–0.35   μg/L. The linear range was 2–2500   μg/L for 17α-ethynylestradiol and 1–2500   μg/L for other estrogens. The relative standard deviations (RSDs) were in the range of 3.7–9.9% ( n   =   8, c   =   20   μg/L) and the enrichment factors were from 30.3 to 55.6-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of estrogens in environmental water samples, and quantitative recoveries were obtained for the spiking experiments.

研究领域: 分析化学 · 环境科学
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CHROMATOGRAPHIA · 2018 ·Vol. 82 ·期 3 ·683-693 · IF 1.401

Hollow Fiber Stir Bar Sorptive Extraction Combined with GC–MS for the Determination of Phthalate Esters from Children’s Food

Shen Chen,Wu Tong,Zang Xiaohuan

In this work, a zeolitic imidazolate framework-based graphene oxide composite (ZIF-8@GO) was prepared and used as the adsorbent in hollow fiber stir bar sorptive extraction. The stir bar was constructed of a small section of hollow fiber filled with 5 mg ZIF-8@GO and a thin stainless wire of 1.5 cm long in its lumen, and used to extract the trace levels of phthalate esters from children’s food samples prior to gas chromatography–mass spectrometric detection. The ZIF-8@GO showed a high adsorption efficiency for the compounds containing aromatic rings. The main experimental parameters that can impact the extraction efficiency including extraction temperature, extraction time, stirring rate, sample salinity, and desorption conditions were investigated. Under the optimized conditions, the limits of detection (LODs) for the five phthalate esters (diethyl phthalate, dipropyl phthalate, diisobutyl phthalate, butylbenzyl phthalate, and di(2-ethylhexyl) phthalate) were 0.15–0.6 µg L −1 for CiCi beverage and pear juice samples, and 0.75–2.2 µg kg −1 for jam samples. The limits of quantitation (LOQs) were 0.5–2.0 µg L −1 for CiCi beverage and pear juice samples, and 2.5–7.5 µg kg −1 for jam samples. Wide linear ranges of 0.5–500.0 µg L −1 and 2.5–2000 µg kg −1 were obtained for CiCi beverage, pear juice samples and jam samples, respectively, with good repeatability (RSD < 11%) and high method recoveries (72%–100%). The lifetime test results showed that the ZIF-8@GO-based hollow fiber stir bar can be reused for 120 extraction cycles without a significant loss of extraction efficiency, indicating its high durability and stability. The established method was applied successfully for the determination of the phthalate esters (PAEs) in children’s food samples. Graphical abstract

研究领域: 分析化学 · 食品安全 · 环境毒理学 · 暴露科学 · 食品化学 · 污染物检测
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FOOD CHEMISTRY · 2024 · IF 8.5

Insight into volatile metabolites and key odorants in black teas processed from Jianghua Kucha tea germplasm (Camellia sinensis var. assamica cv. Jianghua)

Ying-Lin Zhu,Wei-Xuan Li,Yu-Hui Zhang,Han Yan,Long-Yu Guo,Yue Zhang,Hai-Peng Lv,Ling-Hong Zhou,Zhi Lin,Wen-Liang Wu,Yin Zhu

Jianghua Kucha (JHKC) is an ancient tea germplasm, which presents a high value for resource utilization but was less developed in aroma research. In this study, volatile metabolites in fresh leaves and corresponding black teas of JHKC, along with odorants of JHKC black teas were systematically investigated using stir-bar sorptive extraction in combination with gas chromatography–mass spectrometry (GC–MS) and GC–olfactometry/MS (GC–O/MS) technologies. A total of 128 and 135 volatile compounds were identified in fresh leaves and black teas, respectively, along with 13 key differential volatile components derived from fatty acids, pigments, glycoside precursors, and the terpene pathway. An odorant wheel for JHKC black teas was developed based on 29 important odorants determined through a combination of GC–O/MS perception, aroma extract dilution analysis, odor activity value measurement. Trans - β -Damascenone, cis -jasmone, and cis -jasmin lactone have been identified as significant contributors to the “sweet” flavor of JHKC black teas.

研究领域: 农业科学 · 食品科学 · 化学 · 植物科学
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