Mandrah Kapil, Satyanarayana G N V, Roy Somendu Kumar
Analytical Chemistry Laboratory, Regulatory Toxicology Group, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), Vishvigyan Bhavan, 31, Mahatma Gandhi Marg, Lucknow 226001, Uttar Pradesh, India; Academy of Scientific and Innovative Research (AcSIR), CSIR-IITR Campus, Lucknow, India.
Analytical Chemistry Laboratory, Regulatory Toxicology Group, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), Vishvigyan Bhavan, 31, Mahatma Gandhi Marg, Lucknow 226001, Uttar Pradesh, India.
J Chromatogr A. 2017 Dec 15;1528:10-17. doi: 10.1016/j.chroma.2017.10.071. Epub 2017 Oct 28.
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 0.097-100ngmL with coefficients of determination (R)≥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 0.104ngmL and 0.070 to 0.343ngmL, 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.
在本研究中，首次高效开发了一种方法，用于使用分散液液微萃取工艺同时测定瓶装碳酸饮料（从印度勒克瑙当地市场收集）中的九种双酚类似物[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）]。该方法基于漂浮有机液滴固化分散液液微萃取（DLLME-SFO），随后进行进样口硅烷化，并与气相色谱-串联质谱联用。该工艺研究了DLLME-SFO的参数（包括萃取溶剂和分散剂的类型及其体积、pH值、离子强度和样品体积的影响）、影响进样口衍生化的因素，如碰撞能量、进样口温度、衍生化试剂与进样体积以及有机溶剂的类型。每个样品中均检测到了BPA、BPF、BPZ和BPS；而在一些碳酸饮料样品中也检测到了其他双酚。在优化所需条件后，分析物在0.097-100ng/mL范围内具有良好的线性，测定系数（R）≥0.995。该方法的日内和日间精密度良好，相对标准偏差（%RSD）≤10.95%。所有双酚的检测限（LOD）和定量限（LOQ）值分别为0.021至0.104ng/mL和0.070至0.343ng/mL。碳酸饮料样品的萃取回收率良好（73.15-95.08%），富集因子良好（96.36-117.33）。因此，所开发的微萃取方法用于测定瓶装碳酸饮料中的污染物水平具有高度的精确性、快速性和可重复性。
