Li Linqiu, Zhang Xintong, Wang Xin, Qiu Yuan, Li Weiqiao, Guo Lianxian, Shen Qing, Dai Juanxiu
Dongguan Key Laboratory of Public Health Laboratory Science, School of Public Health, Guangdong Medical University, Dongguan, China.
Zhejiang Province Joint Key Laboratory of Aquatic Products Processing, Institute of Seafood, Zhejiang Gongshang University, Hangzhou, China.
Heliyon. 2024 Aug 6;10(16):e35833. doi: 10.1016/j.heliyon.2024.e35833. eCollection 2024 Aug 30.
A rapid high-performance liquid chromatography (HPLC) protocol for the determination of amino acids with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) derivatization was successfully developed for assessing amino acid levels in six species of representative commercial bee pollen. Based on a poroshell column, a favorable chromatographic separation of seventeen amino acids was achieved in approximately 10 min with satisfactory resolution. The LOD and LOQ of this method were less than 0.034 μg/mL and 0.232 μg/mL, and the intra- and inter-day RSDs ranged between 0.86-5.28 % and 3.21-6.50 %, respectively. The matrix effect (ME) ranged from -8 to 3, implying that the matrix effect was not significant. Under the optimum conditions, the established method was adopted to determine amino acids in six types of bee pollens. The results showed that the total amino acid content ranged from 151.94 mg/g () to 214.52 mg/g () in the six bee pollen species. Notably, proline (Pro), valine (Val), leucine (Leu), and phenylalanine (Phe) were abundant in the majority of samples. To identify the suspicious samples, principal component analysis (PCA) was performed, and each type of bee pollen was differentiated. Results showed that, in the market, the qualification rate of was 100 %, but that of was merely 62.5 %, revealing that a few of them were counterfeit. This method offers advantages such as high speed, low cost, and outstanding performance.
建立了一种快速高效液相色谱(HPLC)方法,用于测定6-氨基喹啉-N-羟基琥珀酰亚胺基氨基甲酸酯(AQC)衍生化的氨基酸,以评估6种代表性商业蜂花粉中的氨基酸水平。基于多孔壳柱,在约10分钟内实现了17种氨基酸的良好色谱分离,分离度令人满意。该方法的检测限和定量限分别小于0.034μg/mL和0.232μg/mL,日内和日间相对标准偏差分别在0.86 - 5.28%和3.21 - 6.50%之间。基质效应(ME)在-8至3之间,表明基质效应不显著。在最佳条件下,采用所建立的方法测定了6种蜂花粉中的氨基酸。结果表明,6种蜂花粉中总氨基酸含量在151.94mg/g()至214.52mg/g()之间。值得注意的是,大多数样品中脯氨酸(Pro)、缬氨酸(Val)、亮氨酸(Leu)和苯丙氨酸(Phe)含量丰富。为了识别可疑样品,进行了主成分分析(PCA),并区分了每种蜂花粉。结果显示,市场上的合格率为100%,但的合格率仅为62.5%,表明其中有一些是假冒产品。该方法具有速度快、成本低和性能优异等优点。