China National Tobacco Quality Supervision and Test Center, Zhengzhou, P. R. China.
China tobacco Yunnan Industrial Co. Ltd, Kunming, P. R. China.
J Sep Sci. 2022 Aug;45(15):3043-3053. doi: 10.1002/jssc.202200241. Epub 2022 Jun 22.
A rapid method for determination of parabens preservatives (methyl paraben, ethyl paraben, isopropyl paraben, propyl paraben, isobutyl paraben, and butyl paraben) in flavors was established by using supercritical fluid chromatography-tandem mass spectrometry combined with dispersive solid-phase extraction. After adding methanol and primary secondary amine to the sample simultaneously, high extraction efficiency and good sample cleanup could be obtained by simple shaking. Parabens were well separated on a Chiralpak IG-3 column in 6 min by gradient elution. Recoveries from spiked blank samples at 0.5, 1.0, and 5.0 mg/kg were determined to be 88.3-106.6%with relative standard deviations less than 8.0%. All analytes achieved good linear relation (r ≥ 0.999 2). The limits of detection for all analytes ranged from 0.03 to 0.09 mg/kg and the limits of quantification from 0.11 to 0.31 mg/kg, respectively. A total of 20 actual samples were successfully analyzed by taking the proposed method. Being simple, rapid, green, and reliable, this method can be taken for the determination of parabens preservatives in flavors.
建立了一种超临界流体色谱-串联质谱法结合分散固相萃取快速测定香精中防腐剂(对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸异丙酯、对羟基苯甲酸丙酯、对羟基苯甲酸异丁酯和对羟基苯甲酸丁酯)的方法。样品中同时加入甲醇和仲辛胺,经简单振摇即可实现高提取效率和良好的样品净化。在 Chiralpak IG-3 柱上采用梯度洗脱,6 min 内可实现防腐剂的良好分离。在 0.5、1.0 和 5.0 mg/kg 加标空白样品中的回收率为 88.3%-106.6%,相对标准偏差小于 8.0%。所有分析物均具有良好的线性关系(r ≥ 0.999 2)。所有分析物的检出限为 0.03-0.09 mg/kg,定量限为 0.11-0.31 mg/kg。采用所建立的方法成功分析了 20 个实际样品。该方法简单、快速、绿色、可靠,可用于测定香精中的防腐剂。