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中国精品科技期刊2020
邱月,李根容,陆嘉莉,等. 有机溶剂蛋白质沉淀-高效液相色谱法同时测定乳制品中28种双酚类化合物[J]. 食品工业科技,2025,46(24):1−10. doi: 10.13386/j.issn1002-0306.2025010164.
引用本文: 邱月,李根容,陆嘉莉,等. 有机溶剂蛋白质沉淀-高效液相色谱法同时测定乳制品中28种双酚类化合物[J]. 食品工业科技,2025,46(24):1−10. doi: 10.13386/j.issn1002-0306.2025010164.
QIU Yue, LI Genrong, LU Jiali, et al. Simultaneous Determination of 28 Bisphenols in Dairy Products by Organic Solvent Protein Precipitation Combined with High Performance Liquid Chromatography[J]. Science and Technology of Food Industry, 2025, 46(24): 1−10. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2025010164.
Citation: QIU Yue, LI Genrong, LU Jiali, et al. Simultaneous Determination of 28 Bisphenols in Dairy Products by Organic Solvent Protein Precipitation Combined with High Performance Liquid Chromatography[J]. Science and Technology of Food Industry, 2025, 46(24): 1−10. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2025010164.

有机溶剂蛋白质沉淀-高效液相色谱法同时测定乳制品中28种双酚类化合物

Simultaneous Determination of 28 Bisphenols in Dairy Products by Organic Solvent Protein Precipitation Combined with High Performance Liquid Chromatography

  • 摘要: 基于有机溶剂蛋白质沉淀技术,建立了高效液相色谱(high performance liquid chromatography,HPLC)同时测定乳制品中28种双酚类化合物(bisphenols,BPs)的检测方法,为评估乳制品中BPs的污染风险及食品安全监管提供技术支持。乳制品样品采用含0.1%甲酸的乙腈提取,经冷冻除脂,过0.22 μm聚四氟乙烯滤膜,以0.1%磷酸水-乙腈为流动相,经InfinityLab Poroshell 120 EC-C18柱梯度分离,二极管阵列检测器(diode array detector,DAD)测定,检测波长230 nm,柱温40 ℃,流速1.0 mL/min,进样量10 μL。实验考察了提取溶剂、氯化钠(sodium chloride,NaCl)加入量和提取次数对BPs定量结果的影响。结果表明,17 min内可实现28种BPs的有效分离,28种BPs在各自线性范围内,标准曲线决定系数(R2)均大于0.9990,检出限(limits of detection,LODs)为0.01~0.05 mg/kg,定量限(limits of quantification,LOQs)为0.02~0.10 mg/kg,平均加标回收率为84.2%~103.1%,相对标准偏差(relative standard deviations,RSDs)为0.6%~6.3%。该方法操作简便、快速高效、准确可靠,适用于乳制品中28种BPs的定量检测。

     

    Abstract: A high performance liquid chromatography-diode array detector (HPLC-DAD) method was developed for the simultaneous determination of 28 bisphenols (BPs) in dairy products, based on organic solvent protein precipitation. This method provides technical support for assessing BPs contamination risks and enhancing food safety regulation. The dairy products were extracted with acetonitrile containing 0.1% formic acid, followed by freezing centrifugation for lipid removal, and filtered through 0.22 μm polytetrafluoroethylene (PTFE) membrane. The target analytes were separated on an InfinityLab Poroshell 120 EC-C18 column by a gradient separation using a mixture of 0.1% phosphoric acid and acetonitrile as the mobile phase, and then determined by diode array detector (DAD). The detection wavelength was 230 nm, the column temperature was 40 ℃, the flow rate was 1.0 mL/min, and the injection volume was 10 μL. The experiment investigated the effects of extraction solvent, NaCl addition amount, and extraction cycles on BPs quantification. The results showed that 28 kinds of BPs were effectively separated within 17 min. All 28 BPs demonstrated excellent linearity in their respective concentration ranges, with decision coefficients (R2) exceeding 0.9990 for all calibration curves. The limits of detection (LODs) were 0.01~0.05 mg/kg, the limits of quantification (LOQs) were 0.02~0.10 mg/kg, the average recoveries were 84.2%~103.1%, and the relative standard deviations (RSDs) were 0.6%~6.3% (n=6). The method is convenient, rapid, efficient, accurate and reliable, which is suitable for quantitative detection of 28 BPs in dairy products.

     

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