Advanced Materials Research Chair, Department of Chemistry, College of Science, King Saud University, Riyadh, Kingdom of Saudi Arabia.
J Sep Sci. 2012 Nov;35(21):2892-6. doi: 10.1002/jssc.201200459. Epub 2012 Oct 10.
In the present work, a rapid and sensitive ultra performance liquid chromatography-mass spectrometry method has been proposed for the analysis of capsaicinoids (nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin) present in different Capsicum samples. Extraction of capsaicinoids was carried out by liquid-liquid extraction using ethanol as an extracting solvent, while the chromatographic separation was achieved by reversed phase C(18) column with gradient mobile phase (solvent A: acetonitrile and solvent B: water with 0.1% formic acid). Under the optimum experimental conditions, the linear ranges were 0.5-50 μg/g with correlation coefficient (r(2) ) >0.999 for each capsaicinoids and detection limits were 0.15, 0.05, 0.06, 0.2, and 0.1 μg/g for nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin, respectively. Run-to-run and day-to-day precisions of the method with relative standard deviations <1.5% were achieved for all analyzed capsaicinoids. The robustness of the method was determined by utilizing different injection volumes of the extracts. Furthermore, to validate the system robustness, a run of high number of capsaicinoids present in different varieties of Capsicum samples was performed in this study. All the capsaicinoids were separated in a time of less than 9 min by employing the proposed method.
在本工作中,提出了一种快速灵敏的超高效液相色谱-质谱法,用于分析不同辣椒样品中的辣椒素类物质(降二氢辣椒碱、辣椒素、二氢辣椒碱、高辣椒碱和高二氢辣椒碱)。辣椒素类物质的提取采用液液萃取法,以乙醇为提取溶剂,色谱分离采用反相 C(18)柱,以梯度流动相(溶剂 A:乙腈,溶剂 B:水,含 0.1%甲酸)进行。在最佳实验条件下,各辣椒素类物质的线性范围为 0.5-50μg/g,相关系数(r(2))均大于 0.999,检测限分别为 0.15、0.05、0.06、0.2 和 0.1μg/g。对于所有分析的辣椒素类物质,方法的运行间和日间精密度均以相对标准偏差<1.5%实现。通过利用提取物的不同进样体积来确定方法的稳健性。此外,为了验证系统的稳健性,本研究对不同品种辣椒样品中存在的大量辣椒素类物质进行了一次运行。采用所提出的方法,所有辣椒素类物质在不到 9 分钟的时间内均得到分离。