Development of 1 H-NMR methods for quantitative determination of alkylamides in Zanthoxylum bungeanum and quality evaluation based on its fingerprint.
Development of 1 H-NMR methods for quantitative determination of alkylamides in Zanthoxylum bungeanum and quality evaluation based on its fingerprint.
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建立花椒中烷基酰胺的 1 H-NMR 定量测定方法及基于指纹图谱的质量评价。
DOI：
10.1111/1750-3841.15869
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发表时间：
2021-08
影响因子：
3.9
通讯作者：
Nuernisa Kasimu;Danmeng Yu;Leiwen Sun;Ruofei Zheng;Dongmei Wang
中科院分区：
文献类型：
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作者：
Nuernisa Kasimu;Danmeng Yu;Leiwen Sun;Ruofei Zheng;Dongmei Wang
烷基酰胺类化合物作为花椒的代表性香气成分和活性成分，可以反映花椒的品质。但烷基酰胺中存在共轭三烯结构，在空气中易氧化分解，难以定量。以85%乙醇为最佳萃取溶剂，CDCl 3为最佳氘溶解剂，吡嗪为内标，以δ 6.33ppm处酰胺键上氢质子的三重峰为定量信号峰，建立了1H-NMR技术定量测定烷基酰胺的方法。同时，进行了方法学验证，证明了该方法的可靠性和有效性。在此基础上，得到了9种花椒属植物中烷基酰胺类化合物含量的月变化规律。结果表明，韩城无刺蜂的烷基酰胺类化合物含量较高。8月份花椒含量最高（51.92 ± 0.96 mg/g），6月份花椒含量最低（1.23 ± 0.21 mg/g）。1H-NMR结果与HPLC结果一致，验证了该方法的有效性。积累动态结果表明，玉米的最佳收获期为：bungeanum是七月和八月。此外，还利用所建立的1H-NMR指纹图谱和化学计量学分析对采自普通园林的9个花椒品种进行了质量评价。结果表明，韩城无刺蜂Z.其中，花椒为最佳种质。该研究为Z中烷基酰胺的定量测定提供了一种新的策略。并对花椒的质量评价体系进行了改进。臭牡丹实际应用：该研究结果为枸杞子重要化学成分的分析提供了新的研究思路。臭牡丹同时，该研究也为枣的品质评价和优质种质资源的开发提供了科学依据。臭牡丹
Alkylamides, as the representative hemp flavor and active ingredients, can reflect the quality of Zanthoxylum bungeanum Maxim. However, conjugated triene structure exists in alkylamides, which is easy to be oxidized and decomposed in air, making it difficult to quantify. In this study, a method for the quantitative determination of alkylamides by 1 H-NMR technology was developed with 85% ethanol as the best extraction solvent, CDCl3 as the best deuterium dissolution reagent, pyrazine as the internal standard, and triple peaks of hydrogen protons on the amide bond at δ 6.33 ppm as the quantitative signal peak. Meanwhile, methodological verification was carried out to prove the reliability and effectiveness of the method. On this basis, the contents of alkylamides in nine germplasms of Zanthoxylum with monthly dynamics were obtained. The results showed that the alkylamides of Hancheng stingless Z. bungeanum (HC) exhibited the highest content in August (51.92 ± 0.96 mg/g), while the lowest was FG in June (1.23 ± 0.21 mg/g). The results of 1 H-NMR corresponded to those of HPLC, and the effectiveness of this method was verified. Accumulation dynamic results show that the best harvest period of Z. bungeanum is July and August. Moreover, the quality of nine varieties of Zanthoxylum bungeanum from a common garden was evaluated by the established 1 H-NMR fingerprint and chemometric analyses. The results showed that Hancheng stingless Z. bungeanum was the best germplasm. This study provides a new strategy for the quantitative determination of alkylamides in Z. bungeanum and improves the quality evaluation system of Z. bungeanum. PRACTICAL APPLICATION: The results provide a new research idea for the analysis of important chemical components of Z. bungeanum. Meanwhile, the study provides a scientific basis for the quality evaluation and high-quality germplasm resources of Z. bungeanum.