HPLC-ELSD法测定菊粉中菊粉型果寡糖的含量

doi:10.5246/jcps.2022.01.003

中国药学(英文版) ›› 2022, Vol. 31 ›› Issue (1): 23-30.DOI: 10.5246/jcps.2022.01.003

HPLC-ELSD法测定菊粉中菊粉型果寡糖的含量

崔晓雨¹, 王攀¹, 莫伊点¹, 丁旭阳¹, 陈世忠¹, 郭洪祝², 胡琴²^,^*(), 李中军¹^,^*()

1. 北京大学药学院天然药物及仿生药物国家重点实验室, 北京 100191
2. 北京市药检所 (北京市保健食品化妆品检验中心), 北京 102206

收稿日期:2021-10-11 修回日期:2021-11-05 接受日期:2021-12-21 出版日期:2022-01-12 发布日期:2022-01-13
通讯作者: 胡琴, 李中军
作者简介:
+ Tel.: +86-10-828205939, E-mail: zjli@bjmu.edu.cn
+ Tel.: +86-10-52779622, E-mail: huqin@bidc.org.cn
基金资助:
National Natural Science Foundation of China (Grant No. 21977005) and the Beijing Natural Science Foundation (Grant No. 7192101).

Determination of inulin-type fructo-oligosaccharides in inulin by HPLC-ELSD

Xiaoyu Cui¹, Pan Wang¹, Yidian Mo¹, Xuyang Ding¹, Shizhong Chen¹, Hongzhu Guo², Qin Hu²^,^*(), Zhongjun Li¹^,^*()

1 State Key Laboratory of Natural and Biomimetic Drugs, School of Pharmaceutical Sciences, Peking University Health Science Center, Beijing 100191, China
2 Beijing Institute for Drug Control (Beijing Center for Health Food and Cosmetics Control), Beijing 102206, China

Received:2021-10-11 Revised:2021-11-05 Accepted:2021-12-21 Online:2022-01-12 Published:2022-01-13
Contact: Qin Hu, Zhongjun Li

摘要/Abstract

摘要：

建立HPLC-ELSD法测定菊粉中9种蔗果寡糖的含量, 色谱系统组成: 色谱柱: Waters XBridge^?Amide (4.6 mm × 250 mm, 5 μm); 流动相: CH₃CN–H₂O, 梯度洗脱; 流速: 1.2 mL/min; 柱温: 30 oC; 检测器: Agilent Technologies 380-ELSD, 漂移管温度: 55 oC, N₂流速: 1.8 L/min, 进样量: 15 μL。实验结果是9种菊粉型果寡糖分别在: 蔗果三糖 3.81–30.60 μg, R² = 0.99969; 耐斯糖 3.73–29.97 μg, R² = 0.99981; 蔗果五糖 3.82–30.69 μg, R² = 0.99993; 蔗果六糖3.80–30.48 μg, R²= 0.99995; 蔗果七糖3.73–29.96 μg, R² = 0.99993; 蔗果八糖3.78–30.30 μg, R² = 0.99983; 蔗果九糖3.82–30 μg, R² = 0.99989; 蔗果十糖3.71–29.80 μg, R² = 0.99974; 蔗果十一糖3.61–29.00 μg, R² = 0.99970范围内线性关系良好, 回收率在96.48%–100.84% (n = 6)。该方法简单、准确, 具有良好的重复性, 为有效评价菊粉的质量提供了分析方法。

关键词: 菊粉, 菊粉型果寡糖, 定量检测

Abstract:

To develop an HPLC-ELSD method for the determination of nine inulin-type fructo-oligosaccharides in inulin, the HPLC-ELSD system consisted of Waters XBridge^? Amide column (4.6 mm × 250 mm, 5 μm) with a gradient elution mobile phase consisting of acetonitrile and water at a flow rate of 1.2 mL/min at 30 oC. The detector was an Agilent Technologies 380-ELSD. The drift tube temperature for the ELSD was set at 55 oC with a nitrogen flow rate of 1.8 L/min. The injection volume was 15 μL. The results showed that the detection range for the nine inulin-type fructo-oligosaccharides was 3.81–30.60 μg R²= 0.99969 for kestose, 3.73–29.97 μg R²= 0.99981 for nystose, 3.82–30.69 μg R²= 0.99993 for fructosylnystose, 3.80–30.48 μg R²= 0.99995 for GF₅, 3.73–29.96 μg R²= 0.99993 for GF₆, 3.78–30.30 μg R²= 0.99983 for GF₇, 3.82–30 μg R²= 0.99989 for GF₈, 3.71–29.80 μg R²= 0.99974 for GF₉, 3.61–29.00 μg R²= 0.99970 for GF₁₀, respectively. The recovery of the nine oligosaccharides ranged between 96.48%–100.84% (n = 6). The method was simple, accurate, and reproducible that it could be used as an analytical method for evaluating the quality of inulin effectively.

Key words: Inulin, Inulin-type fructo-oligosaccharides, Quantitative determination

Supporting:

崔晓雨, 王攀, 莫伊点, 丁旭阳, 陈世忠, 郭洪祝, 胡琴, 李中军. HPLC-ELSD法测定菊粉中菊粉型果寡糖的含量[J]. 中国药学(英文版), 2022, 31(1): 23-30.

Xiaoyu Cui, Pan Wang, Yidian Mo, Xuyang Ding, Shizhong Chen, Hongzhu Guo, Qin Hu, Zhongjun Li. Determination of inulin-type fructo-oligosaccharides in inulin by HPLC-ELSD[J]. Journal of Chinese Pharmaceutical Sciences, 2022, 31(1): 23-30.

图/表 7

Figure 1. Structures of inulin-type FOS.

Table 1. Gradient elution table of inulin.

Figure 2. HPLC-ELSD chromatograms of (A) mixed standard stock solution (a), (B) mixed standard stock solution (b), and samples of (C) inulin, (D) Morinda officinalis oligosaccharide capsule, and (E) blank solution.

Table 2. Linear regression data and LOD and LOQ for inulin-type FOS GF2–GF10.

Table 3. Precision, stability, and repeatability for nine inulin-type FOS.

Table 4. Accuracy for inulin-type FOS GF2–GF10.

Table 5. Nine inulin-type FOS contents in two samples.

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HPLC-ELSD法测定菊粉中菊粉型果寡糖的含量

Determination of inulin-type fructo-oligosaccharides in inulin by HPLC-ELSD

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