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Solid phase extraction with high polarity Carb/PSA as composite fillers prior to UPLC-MS/MS to determine six bisphenols and alkylphenols in trace level hotpot seasoning
Food Chemistry ( IF 8.8 ) Pub Date : 2018-03-19 , DOI: 10.1016/j.foodchem.2018.03.074
Hao Dong , Xiaofang Zeng , Weidong Bai

The present study reports an ultra high-performance liquid chromatography tandem mass spectrometry method for the simultaneous determination of six bisphenols (bisphenol A, bisphenol B and bisphenol F) and alkylphenols (4-nonylphenol, 4-n-nonylphenol and octylphenol) in hotpot seasoning. Samples were dispersed in n-hexane after addition of internal standards bisphenol A-d4 and 4-n-nonylphenol-d4. Sample solutions were then centrifuged, and the supernatants purified using solid phase extraction with high polarity Carb/PSA composite fillers. Six target analytes were separated on a Waters ACQUITY BEH C18 column by gradient elution with methanol and 0.05% ammonium hydroxide in water as the mobile phase, and determined under multiple reactions monitoring mode. The limits of detection and quantitation, matrix effect, recovery and precision of the method were investigated. Results were linear in the concentration range 0.1–250 µg/L for all compounds of interest, with R2 > 0.9950. Limits of detection were in the range 0.1–0.4 μg/kg, and limits of quantitation were between 0.5 μg/kg and 1.0 μg/kg. The mean recoveries for negative samples at three spiked concentrations were in the range 87.9%–102.4%, and the intra-day precision and inter-day precision were in the ranges 2.1–8.2% and 4.8–11.2%, respectively. This method is accurate and sensitive, and had good clean-up characteristics, which might apply to screening and quantitation of target bisphenols and alkylphenols in hotpot seasoning.



中文翻译:

在进行UPLC-MS / MS之前,以高极性Carb / PSA作为复合填料进行固相萃取,以确定痕量火锅调味料中的六种双酚和烷基酚

本研究报告了一种超高效液相色谱串联质谱法,用于在火锅调味料中同时测定六种双酚(双酚A,双酚B和双酚F)和烷基酚(4-壬基酚,4-壬基酚和辛基酚) 。样品分散在Ñ正己烷加入内部标准双酚A-后d 4和4- Ñ -nonylphenol- d 4。然后将样品溶液离心,并使用具有高极性Carb / PSA复合填料的固相萃取法纯化上清液。在Waters ACQUITY BEH C18色谱柱上,通过以甲醇和0.05%氢氧化铵水溶液为流动相进行梯度洗脱,分离出六种目标分析物,并在多种反应监测模式下进行测定。研究了该方法的检出限,定量限,基质效应,回收率和精密度。所有目标化合物的浓度范围为0.1–250 µg / L时,结果均为线性,R 2 > 0.9950。检出限在0.1–0.4μg/ kg范围内,定量限在0.5μg/ kg至1.0μg/ kg之间。三种加标浓度的阴性样品的平均回收率在87.9%–102.4%的范围内,日内精度和日间精度分别在2.1–8.2%和4.8–11.2%的范围内。该方法准确,灵敏,净化效果好,可用于火锅调味品中目标双酚和烷基酚的筛选和定量分析。

更新日期:2018-03-19
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