Saaid Mardiana, Saad Bahruddin, Ali Abdussalam Salhin Mohamed, Saleh Muhammad Idiris, Basheer Chanbasha, Lee Hian Kee
School of Chemical Sciences, Universiti Sains Malaysia, 11800 Penang, Malaysia.
J Chromatogr A. 2009 Jul 3;1216(27):5165-70. doi: 10.1016/j.chroma.2009.04.091. Epub 2009 May 3.
Hollow fibre liquid-phase microextraction with in situ derivatization using dansyl chloride has been successfully developed for the high-performance liquid chromatography-ultraviolet (HPLC-UV) determination of the biogenic amines (tryptamine, putrescine, cadaverine, histamine, tyramine, spermidine) in food samples. Parameters affecting the performance of the in situ derivatization process such as type of extraction solvent, temperature, extraction time, stirring speed and salt addition were studied and optimized. Under the optimized conditions (extraction solvent, dihexyl ether; acceptor phase, 0.1M HCl; extraction time, 30 min; extraction temperature, 26 degrees C; without addition of salt), enrichment factors varying from 47 to 456 were achieved. Good linearity of the analytes was obtained over a concentration range of 0.1-5 microg mL(-1) (with correlation coefficients of 0.9901-0.9974). The limits of detection and quantification based on a signal-to-noise ratio of 3-10, ranged from 0.0075 to 0.030 microg mL(-1) and 0.03 to 0.10 microg mL(-1), respectively. The relative standard deviations based on the peak areas for six replicate analysis of water spiked with 0.5 microg mL(-1) of each biogenic amine were lower than 7.5%. The method was successfully applied to shrimp sauce and tomato ketchup samples, offering an interesting alternative to liquid-liquid extraction and solid phase extraction for the analysis of biogenic amines in food samples.
已成功开发出一种采用丹磺酰氯进行原位衍生化的中空纤维液相微萃取方法,用于高效液相色谱 - 紫外(HPLC - UV)测定食品样品中的生物胺(色胺、腐胺、尸胺、组胺、酪胺、亚精胺)。研究并优化了影响原位衍生化过程性能的参数,如萃取溶剂类型、温度、萃取时间、搅拌速度和盐的添加量。在优化条件下(萃取溶剂:二己醚;接受相:0.1M HCl;萃取时间:30分钟;萃取温度:26℃;不添加盐),富集因子在47至456之间。在0.1 - 5μg mL⁻¹的浓度范围内,分析物具有良好的线性关系(相关系数为0.9901 - 0.9974)。基于3 - 10的信噪比,检测限和定量限分别为0.0075至0.030μg mL⁻¹和0.03至0.10μg mL⁻¹。对添加了0.5μg mL⁻¹每种生物胺的水样进行六次重复分析,基于峰面积的相对标准偏差低于7.5%。该方法成功应用于虾酱和番茄酱样品的分析,为食品样品中生物胺的分析提供了一种有趣的替代液 - 液萃取和固相萃取的方法。