College of Food Science and Biotechnology Engineering, Zhejiang Gongshang University, Hangzhou, PR China.
J Sep Sci. 2010 Feb;33(2):235-43. doi: 10.1002/jssc.200900564.
A microwave-assisted extraction (MAE) protocol and an efficient HPLC analysis method were first developed for the fast extraction and simultaneous determination of bisphenol F diglycidyl ether (Novolac glycidyl ether 2-Ring), Novolac glycidyl ether 3-Ring, Novolac glycidyl ether 4-Ring, Novolac glycidyl ether 5-Ring, Novolac glycidyl ether 6-Ring, bisphenol A diglycidyl ether, bisphenol A (2,3-dihydroxypropyl) glycidyl ether, bisphenol A (3-chloro-2-hydroxypropyl) glycidyl ether, bisphenol A bis(3-chloro-2-hydroxypropyl) ether, bisphenol A (3-chloro-2-hydroxypropyl) (2,3-dihydroxypropyl) ether in canned fish and meat. After being optimized in terms of solvents, microwave power and irradiation time, MAE was selected to carry out the extraction of ten target compounds. Analytes were purified by poly(styrene-co-divinylbenzene) SPE columns and determined by HPLC-fluorescence detection. LOD varied from 0.79 to 3.77 ng/g for different target compounds based on S/N=3; LOQ were from 2.75 to 10.92 ng/g; the RSD for repeatability were <8.64%. The analytical recoveries ranged from 70.46 to 103.44%. This proposed method was successfully applied to 16 canned fish and meat, and the results acquired were in good accordance with the studies reported. Compared with the conventional liquid-liquid extraction and ultrasonic extraction, the optimized MAE approach gained the higher extraction efficiency (20-50% improved).
首次开发了一种微波辅助提取(MAE)方案和高效 HPLC 分析方法,用于快速提取和同时测定双酚 F 二缩水甘油醚(Novolac 缩水甘油醚 2-环)、Novolac 缩水甘油醚 3-环、Novolac 缩水甘油醚 4-环、Novolac 缩水甘油醚 5-环、Novolac 缩水甘油醚 6-环、双酚 A 二缩水甘油醚、双酚 A(2,3-二羟基丙基)缩水甘油醚、双酚 A(3-氯-2-羟丙基)缩水甘油醚、双酚 A 双(3-氯-2-羟丙基)醚、双酚 A(3-氯-2-羟丙基)(2,3-二羟基丙基)醚在罐装鱼和肉中的含量。在对溶剂、微波功率和辐照时间进行优化后,选择 MAE 进行十种目标化合物的提取。分析物通过聚苯乙烯-共-二乙烯基苯 SPE 柱纯化,并通过 HPLC-荧光检测进行测定。不同目标化合物的 LOD 范围为 0.79-3.77ng/g(基于 S/N=3);LOQ 范围为 2.75-10.92ng/g;重复性的 RSD 小于 8.64%。分析回收率范围为 70.46-103.44%。该方法成功应用于 16 种罐装鱼和肉,所得结果与已报道的研究结果相符。与传统的液-液萃取和超声萃取相比,优化的 MAE 方法获得了更高的提取效率(提高了 20-50%)。