新疆农业科学 ›› 2022, Vol. 59 ›› Issue (4): 900-907.DOI: 10.6048/j.issn.1001-4330.2022.04.014
金科旭1(), 戴小华1(), 谷虹霏2, 束佳敏1, 王天琪1, 海婷玉1
收稿日期:
2021-03-13
出版日期:
2022-04-20
发布日期:
2022-04-24
通信作者:
戴小华
作者简介:
金科旭(1995-),男,河南鹿邑人,硕士研究生,研究方向为兽医药理,(E-mail) 2212325408@qq.com
基金资助:
JIN Kexu1(), DAI Xiaohua1(), GU Hongfei2, SHU Jiamin1, WANG Tianqi1, HAI Tingyu1
Received:
2021-03-13
Online:
2022-04-20
Published:
2022-04-24
Correspondence author:
DAI Xiaohua
Supported by:
摘要:
【目的】研究优选大孔树脂分离纯化野山杏总黄酮的最佳工艺参数。【方法】采用紫外分光光度法测定野山杏总黄酮含量,利用静态吸附解吸试验分析4种不同型号大孔树脂对野山杏总黄酮的吸附及解吸能力,选出适宜的大孔树脂及其最佳分离纯化条件。【结果】D101型大孔树脂对野山杏总黄酮有较好的比吸附量和解析附能力,最佳分离纯化工艺条件为D-101大孔树脂径高比1∶6,野山杏粗提液最大上样量为6.3 BV,最佳上样浓度为0.3 mg/mL,上样速率为1.0 mL/min,静置时间为2 h,水洗体积为5 BV,水洗液洗脱流速1.5 mL/min,洗脱溶剂用80%乙醇,洗脱溶剂用量2 BV,洗脱剂流速为0.5 mL/min。【结论】D101型大孔树脂在所得工艺条件下可以对野山杏中总黄酮进行较好的分离纯化,可用于野山杏总黄酮的分离纯化。
中图分类号:
金科旭, 戴小华, 谷虹霏, 束佳敏, 王天琪, 海婷玉. 大孔树脂纯化野山杏总黄酮工艺[J]. 新疆农业科学, 2022, 59(4): 900-907.
JIN Kexu, DAI Xiaohua, GU Hongfei, SHU Jiamin, WANG Tianqi, HAI Tingyu. Study on Purification Process of Total Flavonoids from Armeniaca sibirica (L.) Lam by Macroporous Resin[J]. Xinjiang Agricultural Sciences, 2022, 59(4): 900-907.
树脂型号 Resins model | A | 平均值 Average | 比吸附量 Specific adsorption capacity(mg/g) | 比解吸附量 Specific desorption capacity(mg/g) | 解吸率 Desorption rate(%) |
---|---|---|---|---|---|
ADS-17 | 0.263 0.261 0.265 | 0.264 | 1.311 | 0.168 | 12.81 |
D-101 | 0.108 0.111 0.117 | 0.112 | 1.364 | 0.197 | 14.44 |
NAK-9 | 0.269 0.277 0.261 | 0.269 | 1.309 | 0.133 | 10.16 |
AB-8 | 0.198 0.198 0.201 | 0.201 | 1.331 | 0.179 | 13.45 |
表1 4种大孔树脂对野山杏总黄酮静态比吸附量及比解吸量测定
Table 1 Determination of specific adsorption capacity and specific desorption capacity of four kinds of macroporous resins on total flavonoids of Armeniaca sibirica(L.)Lam
树脂型号 Resins model | A | 平均值 Average | 比吸附量 Specific adsorption capacity(mg/g) | 比解吸附量 Specific desorption capacity(mg/g) | 解吸率 Desorption rate(%) |
---|---|---|---|---|---|
ADS-17 | 0.263 0.261 0.265 | 0.264 | 1.311 | 0.168 | 12.81 |
D-101 | 0.108 0.111 0.117 | 0.112 | 1.364 | 0.197 | 14.44 |
NAK-9 | 0.269 0.277 0.261 | 0.269 | 1.309 | 0.133 | 10.16 |
AB-8 | 0.198 0.198 0.201 | 0.201 | 1.331 | 0.179 | 13.45 |
编号 Numbering | 径高比 Ratio of height to height | A | 总黄酮含量 Total flavonoid content(mg/mL) |
---|---|---|---|
1 | 1:4 | 0.468 | 0.035 |
2 | 1:6 | 0.603 | 0.045 |
3 | 1:8 | 0.594 | 0.044 |
表2 径高比变化
Table 2 Inspection results of the ratio of height to height
编号 Numbering | 径高比 Ratio of height to height | A | 总黄酮含量 Total flavonoid content(mg/mL) |
---|---|---|---|
1 | 1:4 | 0.468 | 0.035 |
2 | 1:6 | 0.603 | 0.045 |
3 | 1:8 | 0.594 | 0.044 |
流速 Flow rate (mL/min) | 上样液体积 Sample volume (mL) | 滤液A Filtrate A | 滤液中总 黄酮量 Total flavonoid content in filtrate (mg/mL) | 吸附量 Adsorption capacity (mg/g) |
---|---|---|---|---|
0.5 | 200 | 0.012 | 0.019 4 | 69.98 |
1.0 | 200 | 0.014 | 0.054 8 | 69.95 |
1.5 | 200 | 0.019 | 0.143 4 | 69.86 |
表3 上样流速
Table 3 Sample flow rate
流速 Flow rate (mL/min) | 上样液体积 Sample volume (mL) | 滤液A Filtrate A | 滤液中总 黄酮量 Total flavonoid content in filtrate (mg/mL) | 吸附量 Adsorption capacity (mg/g) |
---|---|---|---|---|
0.5 | 200 | 0.012 | 0.019 4 | 69.98 |
1.0 | 200 | 0.014 | 0.054 8 | 69.95 |
1.5 | 200 | 0.019 | 0.143 4 | 69.86 |
上样浓度 Sample concentration (mg/mL) | 吸光度A Absorbance A | 总黄酮含量 Total flavonoid content (mg/mL) |
---|---|---|
0.1 | 0.206 | 0.016 |
0.2 | 0.389 | 0.029 |
0.3 | 0.565 | 0.042 |
0.4 | 0.403 | 0.030 |
0.5 | 0.371 | 0.028 |
表4 上样浓度
Table 4 Sample Concentration Inspection Results
上样浓度 Sample concentration (mg/mL) | 吸光度A Absorbance A | 总黄酮含量 Total flavonoid content (mg/mL) |
---|---|---|
0.1 | 0.206 | 0.016 |
0.2 | 0.389 | 0.029 |
0.3 | 0.565 | 0.042 |
0.4 | 0.403 | 0.030 |
0.5 | 0.371 | 0.028 |
吸附时间 Adsorption time (h) | 吸光度A Absorbance A | 总黄酮含量 Total flavonoid content (mg/mL) |
---|---|---|
0.5 | 0.317 | 0.024 |
1.0 | 0.364 | 0.027 |
1.5 | 0.375 | 0.028 |
2 | 0.471 | 0.035 |
2.5 | 0.425 | 0.032 |
表5 吸附时间
Table 5 Inspection results of adsorption time
吸附时间 Adsorption time (h) | 吸光度A Absorbance A | 总黄酮含量 Total flavonoid content (mg/mL) |
---|---|---|
0.5 | 0.317 | 0.024 |
1.0 | 0.364 | 0.027 |
1.5 | 0.375 | 0.028 |
2 | 0.471 | 0.035 |
2.5 | 0.425 | 0.032 |
流速 Flow rate(mL/min) | 泄露百分数 Percentage of leaks(%) |
---|---|
0.5 | 1.34 |
1.0 | 1.32 |
1.5 | 1.24 |
表6 水洗脱液流速下泄露百分数
Table 6 Effect of Washing Fluid Flow Rate on Leakage Percentage
流速 Flow rate(mL/min) | 泄露百分数 Percentage of leaks(%) |
---|---|
0.5 | 1.34 |
1.0 | 1.32 |
1.5 | 1.24 |
流速 Flow rate (mL/min) | 洗脱液体积 Elution volume (mL) | 总黄酮含量 Total flavonoid content(mg/mL) |
---|---|---|
0.5 | 160 | 9.446 |
1.0 | 160 | 9.332 |
1.5 | 160 | 9.262 |
表7 洗脱流速考察结果
Table 7 Flow rate of the elution flow
流速 Flow rate (mL/min) | 洗脱液体积 Elution volume (mL) | 总黄酮含量 Total flavonoid content(mg/mL) |
---|---|---|
0.5 | 160 | 9.446 |
1.0 | 160 | 9.332 |
1.5 | 160 | 9.262 |
序号 Numbering | 总黄酮百分含量 Percentage of total flavonoids(%) | 均值 Average(%) |
---|---|---|
1 | 53.11 | |
2 | 51.81 | 52.37 |
3 | 52.18 |
表8 总黄酮含量
Table 8 Total flavonoid content results
序号 Numbering | 总黄酮百分含量 Percentage of total flavonoids(%) | 均值 Average(%) |
---|---|---|
1 | 53.11 | |
2 | 51.81 | 52.37 |
3 | 52.18 |
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