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A dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by injector port silylation coupled with gas chromatography–tandem mass spectrometry for the determination of nine bisphenols in bottled carbonated beverages
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2017-10-28 , DOI: 10.1016/j.chroma.2017.10.071
Kapil Mandrah , G.N.V. Satyanarayana , Somendu Kumar Roy

In the present study, a method has been efficiently developed for the first time to determine nine bisphenol analogues [bisphenol A (BPA), bisphenol C (BPC), bisphenol AF (BPAF), bisphenol E (BPE), bisphenol F (BPF), bisphenol G (BPG), bisphenol M (BPM), bisphenol S (BPS), and bisphenol Z (BPZ)] together in bottled carbonated beverages (collected from the local market of Lucknow, India) using dispersive liquid-liquid microextraction process. This is based on solidification of floating organic droplet (DLLME-SFO) followed by injector port silylation coupled with gas chromatography–tandem mass spectrometry. The process investigated parameters of DLLME-SFO (including the type of extraction and disperser solvents with their volumes, effect of pH, ionic strength, and the sample volume), factors influencing to injection port derivatization like, collision energy, injector port temperature, derivatizing reagent with sample injection volume, and type of organic solvent. BPA, BPF, BPZ, and BPS were detected in each sample; whereas, other bisphenols were also detected in some carbonated beverage samples. After optimizing the required conditions, good linearity of analytes was achieved in the range of 0.097–100 ng mL−1 with coefficients of determination (R2) ≥ 0.995. Intra-day and inter day precision of the method was good, with relative standard deviation (% RSD) ≤ 10.95%. The limits of detection (LOD) and limits of quantification (LOQ) values of all bisphenols were ranged from 0.021 to 0.104 ng mL−1 and 0.070 to 0.343 ng mL−1, respectively. The recovery of extraction was good (73.15–95.08%) in carbonated beverage samples and good enrichment factors (96.36–117.33) were found. Thus, the developed method of microextraction was highly precise, fast, and reproducible to determine the level of contaminants in bottled carbonated beverages.



中文翻译:

基于悬浮有机液滴固化然后进样口甲硅烷基化与气相色谱-串联质谱联用的分散液-液微萃取技术,用于测定瓶装碳酸饮料中的九种双酚

在本研究中,首次有效地开发了一种方法来测定九种双酚类似物[双酚A(BPA),双酚C(BPC),双酚AF(BPAF),双酚E(BPE),双酚F(BPF) ,双酚G(BPG),双酚M(BPM),双酚S(BPS)和双酚Z(BPZ)]一起装在瓶装碳酸饮料中(从印度拉克瑙的本地市场收集),采用分散液-液微萃取工艺。这是基于浮动有机液滴的固化(DLLME-SFO),然后进行进样器端口甲硅烷基化,再结合气相色谱-串联质谱法。该过程研究了DLLME-SFO的参数(包括萃取和分散剂溶剂的类型及其体积,pH值,离子强度和样品体积的影响),影响进样口衍生的因素,例如,碰撞能量,进样口温度,带有进样量的衍生试剂以及有机溶剂的类型。在每个样品中检测到BPA,BPF,BPZ和BPS。而在某些碳酸饮料样品中也检测到其他双酚。优化所需条件后,在0.097–100 ng mL范围内获得了良好的分析物线性-1,确定系数(R 2  ≥0.995。该方法的日内和日间精度良好,相对标准偏差(%RSD)≤10.95%。所有双酚的检出限LOD)和定量LOQ)值分别为0.021至0.104 ng mL -1和0.070至0.343 ng mL -1。在碳酸饮料样品中,提取物的回收率很高(73.15-95.08%),并且富集因子也很高(96.36-117.33)。因此,开发的微萃取方法高度精确,快速且可重现,可测定瓶装碳酸饮料中的污染物含量。

更新日期:2017-10-28
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