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目的:建立柱后衍生阳离子交换色谱方法,测定甘肃紫斑牡丹花粉氨基酸的含量。方法:样品加6 mol·L~(-1)盐酸于110℃水解22 h。采用柱后衍生阳离子交换色谱法,对甘肃产紫斑牡丹花粉氨基酸的含量进行分析;色谱柱:LCAK06/Na型磺酸基强酸性阳离子交换树脂色谱柱(4.6 mm×150 mm,5μm),梯度洗脱,其中A泵(溶液泵)流速为0.45 m L·min~(-1),M泵(茚三酮泵)流速为0.25 m L·min~(-1),检测波长为440 nm(脯氨酸)和570 nm(其余氨基酸),进样量为50μL。结果:该测定方法中天冬氨酸、苏氨酸、丝氨酸、谷氨酸、脯氨酸、甘氨酸、丙氨酸、胱氨酸、缬氨酸、蛋氨酸、异亮氨酸、亮氨酸、酪氨酸、苯丙氨酸、组氨酸、赖氨酸、精氨酸的线性关系良好;精密度RSD范围为0.10%~1.6%,重复性RSD范围为0.20%~1.5%;平均回收率(n=6)在89.5%~98.2%之间,RSD在0.81%~2.9%之间。样品中所含氨基酸的范围为4.13~44.23 mg·g~(-1),破壁前后所测得氨基酸含量无显著差异。结论:所建立的分析方法可作为紫斑牡丹花粉中氨基酸的定量分析。
OBJECTIVE: To establish a post-column derivatization cation exchange chromatography method for determination of amino acids in pollen of Gansu purpurea. Methods: Samples were hydrolyzed with 6 mol·L ~ (-1) HCl at 110 ℃ for 22 h. The post-column derivatization cation exchange chromatography was used to analyze the contents of amino acids in pollens from Gansu Province. The chromatographic column (4.6 mm × 150 mm, 5 μm) of LCAK06 / Na sulfonic acid-based strong acid cation exchange resin The flow rate of A pump (solution pump) was 0.45 m L · min -1, that of M pump (ninhydrin pump) was 0.25 m L · min -1, and the detection wavelength was 440 nm Amino acid) and 570 nm (the remaining amino acids), injection volume of 50μL. Results: Aspartic acid, threonine, serine, glutamic acid, proline, glycine, alanine, cystine, valine, methionine, isoleucine, leucine, The linear relationship between tyrosine, phenylalanine, histidine, lysine and arginine was good. The RSD range of precision was 0.10% ~ 1.6% and the range of RSD was 0.20% ~ 1.5%. The average recovery (n = 6) ranged from 89.5% to 98.2% and RSD ranged from 0.81% to 2.9%. The amino acids contained in the sample ranged from 4.13 to 44.23 mg · g -1. There was no significant difference in amino acid content before and after the breakage. Conclusion: The established analytical method can be used as a quantitative analysis of amino acids in the purple peony pollen.