浙江农业学报 ›› 2026, Vol. 38 ›› Issue (6): 1153-1163.DOI: 10.3969/j.issn.1004-1524.20250529
韦丽萍1(
), 王阳光1,*(
), 杨英1, 陆胜民2,*(
)
收稿日期:2025-08-11
出版日期:2026-06-25
发布日期:2026-07-14
作者简介:韦丽萍,研究方向为食品加工与安全。E-mail:2293613854@qq.com
通讯作者:
*王阳光,E-mail:634449563@qq.com;陆胜民,E-mail:1010508971@qq.com
基金资助:
WEI Liping1(
), WANG Yangguang1,*(
), YANG Ying1, LU Shengmin2,*(
)
Received:2025-08-11
Published:2026-06-25
Online:2026-07-14
摘要:
为高效提取胡柚青果干(衢枳壳原料)中富含的柚皮苷和新橙皮苷,本研究采用超声辅助乙醇浸提法进行单因素同步提取实验,并通过响应面法进行优化;选用AB-8大孔吸附树脂对粗提物进行纯化,并对纯化前后的提取物进行体外抗氧化和降糖活性比较。结果表明,在乙醇体积分数43%、超声时间14 min、超声功率300 W、料液比1∶16(g·mL-1)条件下,柚皮苷和新橙皮苷的提取得率分别为133.19 mg·g-1和99.23 mg·g-1,总得率为232.42 mg·g-1;纯化后提取物中柚皮苷和新橙皮苷的纯度分别提高了2.47和1.74百分点,且DPPH自由基清除率、ABTS自由基清除率和α-葡萄糖苷酶抑制率均显著(p<0.05)提高。以上研究表明,该提取和纯化工艺简单、有效,且所得提取物具有较好的功能活性,为胡柚青果中活性成分的高效提取和利用提供了技术基础。
中图分类号:
韦丽萍, 王阳光, 杨英, 陆胜民. 胡柚青果干中柚皮苷和新橙皮苷的同步提取、纯化及其功能活性分析[J]. 浙江农业学报, 2026, 38(6): 1153-1163.
WEI Liping, WANG Yangguang, YANG Ying, LU Shengmin. Synchronous extraction, purification, and functional activity analysis of naringin and neohesperidin from dried immature Huyou (Citrus ×aurantium Changshanhuyou) fruits[J]. Acta Agriculturae Zhejiangensis, 2026, 38(6): 1153-1163.
图2 单因素水平对胡柚青果干柚皮苷(NR)和新橙皮苷(NHP)得率的影响 NR,柚皮苷;NHP,新橙皮苷。无相同小写字母表示差异显著(p<0.05)。
Fig.2 Effects of single factor levels on yield of naringin(NR) and neohesperidin(NHP) from dried immature Huyou (Citrus×aurantium Changshanhuyou) fruit NR, Naringin; NHP, Neohesperidin. Values marked without the same lowercase letter indicates significant (p<0.05) differences.
| 水平 Level | A/% | B/min | C/W | D/(g·mL-1) |
|---|---|---|---|---|
| -1 | 20 | 5 | 250 | 1∶5 |
| 0 | 40 | 15 | 300 | 1∶15 |
| 1 | 60 | 25 | 350 | 1∶25 |
表1 响应面实验的因素与水平
Table 1 Factors and levels used in response surface analysis
| 水平 Level | A/% | B/min | C/W | D/(g·mL-1) |
|---|---|---|---|---|
| -1 | 20 | 5 | 250 | 1∶5 |
| 0 | 40 | 15 | 300 | 1∶15 |
| 1 | 60 | 25 | 350 | 1∶25 |
| A/% | B/min | C/W | D/(g·mL-1) | NR得率/(mg·g-1) NR yield/(mg·g-1) | NHP得率/(mg·g-1) NHP yield/(mg·g-1) | 总得率/(mg·g-1) Total yield/(mg·g-1) |
|---|---|---|---|---|---|---|
| 40 | 15 | 250 | 1∶25 | 94.08 | 74.14 | 168.22 |
| 20 | 25 | 300 | 1∶15 | 82.70 | 68.65 | 151.35 |
| 40 | 15 | 350 | 1∶25 | 104.07 | 91.99 | 196.06 |
| 40 | 5 | 300 | 1∶5 | 83.66 | 72.33 | 155.99 |
| 60 | 25 | 300 | 1∶15 | 94.49 | 80.31 | 174.80 |
| 20 | 5 | 300 | 1∶15 | 85.43 | 73.90 | 159.33 |
| 20 | 15 | 300 | 1∶5 | 89.71 | 74.59 | 164.30 |
| 40 | 15 | 300 | 1∶15 | 132.79 | 98.10 | 230.89 |
| 40 | 25 | 250 | 1∶15 | 81.11 | 66.26 | 147.37 |
| 40 | 25 | 300 | 1∶25 | 91.24 | 72.87 | 164.11 |
| 40 | 5 | 300 | 1∶25 | 98.34 | 78.82 | 177.16 |
| 40 | 25 | 350 | 1∶15 | 81.96 | 73.43 | 155.39 |
| 60 | 15 | 250 | 1∶15 | 96.46 | 80.33 | 176.79 |
| 60 | 15 | 350 | 1∶15 | 110.83 | 77.21 | 188.04 |
| 40 | 5 | 350 | 1∶15 | 95.42 | 77.59 | 173.01 |
| 60 | 15 | 300 | 1∶5 | 93.46 | 68.66 | 162.12 |
| 40 | 15 | 350 | 1∶5 | 90.61 | 79.11 | 169.72 |
| 40 | 5 | 250 | 1∶15 | 83.83 | 68.49 | 152.32 |
| 20 | 15 | 350 | 1∶15 | 88.97 | 79.63 | 168.60 |
| 40 | 15 | 300 | 1∶15 | 135.65 | 104.23 | 239.88 |
| 40 | 15 | 300 | 1∶15 | 130.03 | 104.18 | 234.21 |
| 60 | 15 | 300 | 1∶25 | 98.87 | 88.90 | 187.77 |
| 20 | 15 | 250 | 1∶15 | 84.53 | 74.54 | 159.07 |
| 40 | 15 | 300 | 1∶15 | 128.65 | 101.60 | 230.25 |
| 40 | 25 | 300 | 1∶5 | 83.93 | 74.68 | 158.61 |
| 20 | 15 | 300 | 1∶25 | 88.38 | 71.13 | 159.52 |
| 40 | 15 | 250 | 1∶5 | 89.83 | 80.01 | 169.84 |
| 60 | 5 | 300 | 1∶15 | 100.86 | 82.47 | 183.33 |
| 40 | 15 | 300 | 1∶15 | 130.89 | 105.68 | 236.57 |
表2 响应面实验结果
Table 2 Response surface test results
| A/% | B/min | C/W | D/(g·mL-1) | NR得率/(mg·g-1) NR yield/(mg·g-1) | NHP得率/(mg·g-1) NHP yield/(mg·g-1) | 总得率/(mg·g-1) Total yield/(mg·g-1) |
|---|---|---|---|---|---|---|
| 40 | 15 | 250 | 1∶25 | 94.08 | 74.14 | 168.22 |
| 20 | 25 | 300 | 1∶15 | 82.70 | 68.65 | 151.35 |
| 40 | 15 | 350 | 1∶25 | 104.07 | 91.99 | 196.06 |
| 40 | 5 | 300 | 1∶5 | 83.66 | 72.33 | 155.99 |
| 60 | 25 | 300 | 1∶15 | 94.49 | 80.31 | 174.80 |
| 20 | 5 | 300 | 1∶15 | 85.43 | 73.90 | 159.33 |
| 20 | 15 | 300 | 1∶5 | 89.71 | 74.59 | 164.30 |
| 40 | 15 | 300 | 1∶15 | 132.79 | 98.10 | 230.89 |
| 40 | 25 | 250 | 1∶15 | 81.11 | 66.26 | 147.37 |
| 40 | 25 | 300 | 1∶25 | 91.24 | 72.87 | 164.11 |
| 40 | 5 | 300 | 1∶25 | 98.34 | 78.82 | 177.16 |
| 40 | 25 | 350 | 1∶15 | 81.96 | 73.43 | 155.39 |
| 60 | 15 | 250 | 1∶15 | 96.46 | 80.33 | 176.79 |
| 60 | 15 | 350 | 1∶15 | 110.83 | 77.21 | 188.04 |
| 40 | 5 | 350 | 1∶15 | 95.42 | 77.59 | 173.01 |
| 60 | 15 | 300 | 1∶5 | 93.46 | 68.66 | 162.12 |
| 40 | 15 | 350 | 1∶5 | 90.61 | 79.11 | 169.72 |
| 40 | 5 | 250 | 1∶15 | 83.83 | 68.49 | 152.32 |
| 20 | 15 | 350 | 1∶15 | 88.97 | 79.63 | 168.60 |
| 40 | 15 | 300 | 1∶15 | 135.65 | 104.23 | 239.88 |
| 40 | 15 | 300 | 1∶15 | 130.03 | 104.18 | 234.21 |
| 60 | 15 | 300 | 1∶25 | 98.87 | 88.90 | 187.77 |
| 20 | 15 | 250 | 1∶15 | 84.53 | 74.54 | 159.07 |
| 40 | 15 | 300 | 1∶15 | 128.65 | 101.60 | 230.25 |
| 40 | 25 | 300 | 1∶5 | 83.93 | 74.68 | 158.61 |
| 20 | 15 | 300 | 1∶25 | 88.38 | 71.13 | 159.52 |
| 40 | 15 | 250 | 1∶5 | 89.83 | 80.01 | 169.84 |
| 60 | 5 | 300 | 1∶15 | 100.86 | 82.47 | 183.33 |
| 40 | 15 | 300 | 1∶15 | 130.89 | 105.68 | 236.57 |
| 方差来源 Source of variance | 平方和 Sum of squares | 自由度 Degrees of freedom | 均方 Mean square | F值 F value | p |
|---|---|---|---|---|---|
| 模型Model | 21 700.21 | 14 | 1 550.02 | 45.43 | <0.000 1 |
| A | 1 020.84 | 1 | 1 020.84 | 29.92 | <0.000 1 |
| B | 204.27 | 1 | 204.27 | 5.99 | 0.028 2 |
| C | 496.78 | 1 | 496.78 | 14.56 | 0.001 9 |
| D | 435.13 | 1 | 435.13 | 12.75 | 0.003 1 |
| AB | 0.08 | 1 | 0.08 | 2.22×10-3 | 0.963 1 |
| AC | 0.74 | 1 | 0.74 | 0.02 | 0.885 0 |
| AD | 231.50 | 1 | 231.50 | 6.78 | 0.020 8 |
| BC | 40.13 | 1 | 40.13 | 1.18 | 0.296 4 |
| BD | 61.39 | 1 | 61.39 | 1.80 | 0.201 2 |
| CD | 195.44 | 1 | 195.44 | 5.73 | 0.031 3 |
| A2 | 6 002.44 | 1 | 6 002.44 | 175.92 | <0.000 1 |
| B2 | 10 745.46 | 1 | 10 745.46 | 314.94 | <0.000 1 |
| C2 | 6 536.21 | 1 | 6 536.21 | 191.57 | <0.000 1 |
| D2 | 6 081.63 | 1 | 6 081.63 | 178.25 | <0.000 1 |
| 残差Residual | 477.67 | 14 | 34.12 | — | — |
| 失拟项Lack of fit | 413.36 | 10 | 41.34 | 2.57 | 0.188 0 |
| 纯误差Pure error | 64.31 | 4 | 16.08 | — | — |
| 总回归Total regression | 22 177.88 | 28 | — | — | — |
表3 回归模型的方差分析
Table 3 Analysis of variance for the regression model
| 方差来源 Source of variance | 平方和 Sum of squares | 自由度 Degrees of freedom | 均方 Mean square | F值 F value | p |
|---|---|---|---|---|---|
| 模型Model | 21 700.21 | 14 | 1 550.02 | 45.43 | <0.000 1 |
| A | 1 020.84 | 1 | 1 020.84 | 29.92 | <0.000 1 |
| B | 204.27 | 1 | 204.27 | 5.99 | 0.028 2 |
| C | 496.78 | 1 | 496.78 | 14.56 | 0.001 9 |
| D | 435.13 | 1 | 435.13 | 12.75 | 0.003 1 |
| AB | 0.08 | 1 | 0.08 | 2.22×10-3 | 0.963 1 |
| AC | 0.74 | 1 | 0.74 | 0.02 | 0.885 0 |
| AD | 231.50 | 1 | 231.50 | 6.78 | 0.020 8 |
| BC | 40.13 | 1 | 40.13 | 1.18 | 0.296 4 |
| BD | 61.39 | 1 | 61.39 | 1.80 | 0.201 2 |
| CD | 195.44 | 1 | 195.44 | 5.73 | 0.031 3 |
| A2 | 6 002.44 | 1 | 6 002.44 | 175.92 | <0.000 1 |
| B2 | 10 745.46 | 1 | 10 745.46 | 314.94 | <0.000 1 |
| C2 | 6 536.21 | 1 | 6 536.21 | 191.57 | <0.000 1 |
| D2 | 6 081.63 | 1 | 6 081.63 | 178.25 | <0.000 1 |
| 残差Residual | 477.67 | 14 | 34.12 | — | — |
| 失拟项Lack of fit | 413.36 | 10 | 41.34 | 2.57 | 0.188 0 |
| 纯误差Pure error | 64.31 | 4 | 16.08 | — | — |
| 总回归Total regression | 22 177.88 | 28 | — | — | — |
图3 胡柚青果干NR和NHP的3D响应面图 A,乙醇体积分数;B,超声时间;C,超声功率;D,料液比。
Fig.3 3D Response surface of NR and NHP from dried immature Huyou (Citrus×aurantium Changshanhuyou) fruit A, Ethanol volume fraction; B, Ultrasonic time; C, Ultrasonic power; D, Solid?liquid ratio.
| 树脂种类 Resin type | NR吸附率 NR adsorption rate | NR解吸率 NR desorption rate | NHP吸附率 NHP adsorption rate | NHP解吸率 NHP desorption rate |
|---|---|---|---|---|
| AB-8 | 91.26±0.18 a | 62.12±2.89 a | 92.86±0.15 a | 62.01±2.91 a |
| D101 | 86.03±0.36 c | 62.46±2.28 a | 88.03±0.32 c | 63.55±3.01 a |
| HPD-100 | 89.25±0.12 b | 63.36±3.09 a | 91.03±0.09 b | 62.56±3.78 a |
| HPD-300 | 82.77±0.72 d | 62.32±3.70 a | 84.97±0.58 d | 62.65±2.63 a |
表4 各种树脂的极性及其对NR和NHP的吸附率和解吸率
Table 4 Polarity of various resins and their adsorption and desorption rates for NR and NHP
| 树脂种类 Resin type | NR吸附率 NR adsorption rate | NR解吸率 NR desorption rate | NHP吸附率 NHP adsorption rate | NHP解吸率 NHP desorption rate |
|---|---|---|---|---|
| AB-8 | 91.26±0.18 a | 62.12±2.89 a | 92.86±0.15 a | 62.01±2.91 a |
| D101 | 86.03±0.36 c | 62.46±2.28 a | 88.03±0.32 c | 63.55±3.01 a |
| HPD-100 | 89.25±0.12 b | 63.36±3.09 a | 91.03±0.09 b | 62.56±3.78 a |
| HPD-300 | 82.77±0.72 d | 62.32±3.70 a | 84.97±0.58 d | 62.65±2.63 a |
图4 胡柚青果干NR和NHP提取物纯化前后的抗氧化活性 无相同小写字母表示相同质量浓度下不同样品对自由基清除能力差异显著(p<0.05)。下同。
Fig.4 Antioxidant activities of NR and NHP extracts from dried immature Huyou (Citrus×aurantium Changshanhuyou) fruit before and after purification Dots marked without the same lowercase letters indicate significant (p<0.05) differences in free radical scavenging capacity among samples at the same mass concentration. The same as below.
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