Hughey Christine A, Wilcox Bruce, Minardi Carina S, Takehara Chiyo W, Sundararaman Meenakshi, Were Lilian M
Department of Chemistry, Chapman University, 1 University Drive, Orange, CA 92866, United States.
J Chromatogr A. 2008 May 30;1192(2):259-65. doi: 10.1016/j.chroma.2008.03.079. Epub 2008 Apr 3.
A rapid negative ion ESI high-performance capillary liquid chromatography-mass spectrometry method was developed to identify and quantify flavonoids (e.g., flavanols, flavonols, flavanones and glycosides). Fifteen standards and two varieties of almond skin extract powder (Carmel and Nonpareil) were used to demonstrate the chromatographic separation, reproducibility and accuracy of the method that employed a 150 mm x 0.3 mm ChromXP 3C18-EP-120 column. All standards eluted in less than 10 min, providing a 9-12x reduction in analysis time compared to existing methods (90-120 min). However, isomers (e.g., catechin/epicatechin and galactosides/glucosides) were not resolved and, therefore, identified and quantified collectively. RSDs for retention time and peak area reproducibility (mass spectrometry data) were <0.5% and <5.0%, respectively. Peak area reproducibility was greatly improved (from a RSD>10%) after the implementation of a low-flow metal needle in the ESI source. Quantitation by mass spectrometry also afforded a % error less than 5% for most compounds.
建立了一种快速负离子电喷雾电离高效毛细管液相色谱 - 质谱法,用于鉴定和定量黄酮类化合物(如黄烷醇、黄酮醇、黄烷酮和糖苷)。使用15种标准品以及两种杏仁皮提取物粉末(卡梅尔和无与伦比)来证明该方法的色谱分离效果、重现性和准确性,该方法采用150 mm×0.3 mm ChromXP 3C18 - EP - 120色谱柱。所有标准品在不到10分钟内洗脱完毕,与现有方法(90 - 120分钟)相比,分析时间减少了9 - 12倍。然而,异构体(如儿茶素/表儿茶素和半乳糖苷/葡萄糖苷)未得到分离,因此进行了集体鉴定和定量。保留时间和峰面积重现性(质谱数据)的相对标准偏差分别<0.5%和<5.0%。在电喷雾电离源中采用低流量金属针后,峰面积重现性得到了极大改善(相对标准偏差从>10%降低)。大多数化合物通过质谱法定量的误差百分比也小于5%。