Machonis Philip, Jones Matthew, Schaneberg Brian, Kwik-Uribe Catherine, Dowell Dawn
J AOAC Int. 2014 Mar-Apr;97(2):506-9. doi: 10.5740/jaoacint.13-351.
Single-laboratory validation data previously published in the Journal of AOAC INTERNATIONAL 95(2), 500-507 (2012) was reviewed by the Stakeholder Panel on Strategic Food Analytical Methods Expert Review Panel (ERP) at the AOAC INTERNATIONAL Mid-Year Meeting held on March 12-14, 2013 in Rockville, MD. The ERP determined the data presented met the established standard method performance requirement and approved the method as AOAC Official First Action on March 14, 2013. Using high-performance liquid chromatography (HPLC), flavanol enantiomers, (+)- and (-)-epicatechin and (+)- and (-)-catechin, are eluted isocratically using ammonium acetate and methanol mobile phase. The mobile phase is applied to a modified beta-cyclodextrin chiral stationary phase and the flavanols detected by fluorescence. Using several cocoa-based matrices, recoveries for the four enantiomers ranged from 82.2-102.1% at a 50% spike level, and 80.4-101.1% at a 100% spike level. Precision was determined to be 1.46-3.22% for (-)-epicatechin, 3.66-6.90% for (+)-catechin, 1.69-6.89% for (-)-catechin. (+)-Epicatechin was not detected in any of the samples used for this work, so precision could not be determined for this molecule.
之前发表于《美国官方分析化学家协会国际期刊》95(2), 500 - 507 (2012)的单实验室验证数据,在2013年3月12 - 14日于马里兰州罗克维尔举行的美国官方分析化学家协会年中会议上,由战略食品分析方法专家评审小组(ERP)进行了评审。ERP判定所呈现的数据符合既定的标准方法性能要求,并于2013年3月14日批准该方法为美国官方分析化学家协会首次行动方法。使用高效液相色谱法(HPLC),黄烷醇对映体,(+)-和(-)-表儿茶素以及(+)-和(-)-儿茶素,使用醋酸铵和甲醇流动相进行等度洗脱。流动相应用于改性β-环糊精手性固定相,黄烷醇通过荧光检测。使用几种基于可可的基质,四种对映体在50%加标水平下的回收率为82.2 - 102.1%,在100%加标水平下的回收率为80.4 - 101.1%。(-)-表儿茶素的精密度测定为1.46 - 3.22%,(+)-儿茶素为3.66 - 6.90%,(-)-儿茶素为1.69 - 6.89%。在本研究使用的任何样品中均未检测到(+)-表儿茶素,因此无法确定该分子的精密度。