林产化学与工业 ›› 2022, Vol. 42 ›› Issue (2): 115-124.doi: 10.3969/j.issn.0253-2417.2022.02.016
收稿日期:
2021-06-27
出版日期:
2022-04-28
发布日期:
2022-05-06
通讯作者:
王冬梅
E-mail:971788137@qq.com;dmwli@163.com
作者简介:
王冬梅, 教授, 博士生导师, 研究领域为特色林源活性物质分离、结构鉴定及其应用; E-mail: dmwli@163.com基金资助:
Ruofei ZHENG(), Zijia LIU, Nuernisa KASIMU, Dongmei WANG(
)
Received:
2021-06-27
Online:
2022-04-28
Published:
2022-05-06
Contact:
Dongmei WANG
E-mail:971788137@qq.com;dmwli@163.com
摘要:
以花椒叶与金露梅叶为原料,采用超声波辅助提取联合大孔树脂吸附技术制备花椒叶提取物(ZBE)与金露梅叶提取物(PFE),通过等辐射分析法研究二者的抗氧化协同效应,确定其最佳复配比;采用单因素试验与正交试验确定花椒叶-金露梅叶复合饮料的生产配方与制备工艺。研究结果表明:当ZEB与PFE复配比为3:1(质量比)时,其抗氧化协同效应最强。复合饮料的最佳配方为花椒叶-金露梅叶复配物(3:1)0.1%、木糖醇0.015%、阿斯巴甜8.00%、柠檬酸0.10%、CMC-Na 0.30%、黄原胶0.02%、β-环状糊精0.40%和山梨酸钾0.05%。煮沸灭菌30 min后,饮料的菌落总数、霉菌、酵母菌、大肠杆菌数与食源性致病菌数符合国家标准;总酚的量(TFC)为0.014 1 μmol/g,总黄酮的量(TPC)为0.019 8 μmol/g,6种主要成分儿茶素、阿魏酸、金丝桃苷、芦丁、槲皮苷和阿福豆苷的量分别为(28.76±0.20)、(13.72±0.16)、(65.32±0.55)、(19.85±0.27)、(62.76±0.36)、(16.78±0.22) mg/g;ABTS+·清除能力为(2.09±0.011)μmol/g,三价铁离子还原能力(FRAP)为(1.21±0.003)μmol/g,DPPH·的半数抑制质量浓度(IC50)为(436.48±3.16) mg/L,具有较强的抗氧化活性。化学稳定性试验与保质期的预测及验证试验表明,该饮料在(25±2)℃下保质期可达6个月。
中图分类号:
郑若菲, 刘子嘉, 努尔尼萨·喀斯木, 王冬梅. 花椒叶-金露梅叶复合饮料的制备及其抗氧化活性研究[J]. 林产化学与工业, 2022, 42(2): 115-124.
Ruofei ZHENG, Zijia LIU, Nuernisa KASIMU, Dongmei WANG. Preparation and Antioxidant Effect of Zanthoxylum bungeanum Leaves and Potentilla fruticosa Leaves Extracts Compound Beverage[J]. Chemistry and Industry of Forest Products, 2022, 42(2): 115-124.
表2
不同比例复配物中活性成分含量1)"
mZBE: mPFE | TPC/(μmol·g-1) | TFC/(μmol·g-1) | CAT/(mg·g-1) | FER/(mg·g-1) | HYD/(mg·g-1) | RUT/(mg·g-1) | QUE/(mg·g-1) | AFZ/(mg·g-1) |
1:0 | 1.9231±0.0087 | 2.2596±0.0359 | — | — | 124.39±3.93 | 38.57±1.31 | 125.74±5.52 | 33.76±0.97 |
0:1 | 1.6135±0.0095 | 2.3309±0.0201 | 110.97±2.44 | 36.09±1.77 | — | — | — | — |
2:1 | 1.7805±0.0087 | 2.3070±0.0109 | 42.53±2.63 | 17.24±0.49 | 73.42±2.00 | 22.46±1.31 | 71.12±1.85 | 15.38±0.44 |
3:1 | 1.8432±0.0144 | 2.2881±0.0145 | 36.23±1.91 | 15.34±0.34 | 75.21±1.30 | 25.43±0.51 | 75.77±2.25 | 21.52±0.49 |
4:1 | 1.8489±0.0066 | 2.2691±0.0055 | 24.87±1.44 | 8.75±0.21 | 86.75±2.15 | 31.56±0.75 | 85.29±2.17 | 25.33±0.95 |
5:1 | 1.8946±0.0087 | 2.2596±0.0095 | 17.41±0.62 | 6.75±0.07 | 95.32±2.13 | 33.89±1.47 | 94.27±2.24 | 28.47±1.61 |
表3
ZBE和PFE复配物添加量的确定"
添加量/% addition | TPC/(μmol·g-1) | TFC/(μmol·g-1) | RABTS+·/(μmol·g-1) | RFRAP/(μmol·g-1) | IC50, DPPH·/(mg·L-1) |
0.05 | 0.0102 | 0.0153 | 1.74±0.009 | 0.85±0.010 | 3.54±0.05 |
0.10 | 0.0157 | 0.0215 | 2.37±0.011 | 1.37±0.008 | 3.22±0.07 |
0.15 | 0.0187 | 0.0258 | 2.91±0.012 | 1.76±0.007 | 3.15±0.08 |
0.20 | 0.0223 | 0.0302 | 3.36±0.015 | 2.11±0.008 | 3.28±0.08 |
表4
正交试验的极差分析"
试验号 No. | A | B | C | 沉降率/% sedimentation rate | 试验号 No. | A | B | C | 得分 score | |
羧甲基纤维素钠/% CMC-Na | 黄原胶/% xanthan gum | β-环状糊精/% β-cyclodextrin | 阿斯巴甜/% aspartame | 木糖醇/% xylitol | 柠檬酸/% citric acid | |||||
1 | 0.20 | 0.02 | 0.40 | 1.08 | 1 | 6.00 | 0.005 | 0.05 | 75.07 | |
2 | 0.20 | 0.03 | 0.50 | 2.76 | 2 | 6.00 | 0.010 | 0.10 | 78.62 | |
3 | 0.20 | 0.04 | 0.60 | 2.58 | 3 | 6.00 | 0.015 | 0.15 | 78.19 | |
4 | 0.25 | 0.02 | 0.60 | 2.16 | 4 | 7.00 | 0.005 | 0.15 | 77.92 | |
5 | 0.25 | 0.03 | 0.40 | 2.01 | 5 | 7.00 | 0.010 | 0.05 | 74.86 | |
6 | 0.25 | 0.04 | 0.50 | 2.52 | 6 | 7.00 | 0.015 | 0.10 | 76.98 | |
7 | 0.30 | 0.02 | 0.50 | 0.92 | 7 | 8.00 | 0.005 | 0.10 | 78.69 | |
8 | 0.30 | 0.03 | 0.60 | 1.80 | 8 | 8.00 | 0.010 | 0.15 | 77.65 | |
9 | 0.30 | 0.04 | 0.40 | 2.62 | 9 | 8.00 | 0.015 | 0.05 | 80.43 | |
k1 | 2.14 | 1.39 | 1.90 | k1 | 77.29 | 77.23 | 76.79 | |||
k2 | 2.23 | 2.19 | 2.07 | k2 | 76.59 | 77.04 | 78.10 | |||
k3 | 1.78 | 2.57 | 2.18 | k3 | 78.92 | 78.53 | 77.92 | |||
R | 0.45 | 1.18 | 0.28 | R | 2.33 | 1.49 | 1.31 |
表5
不同灭菌工艺的灭菌效果1)"
灭菌工艺 treatment | 菌落总数/(CFU·mL-1) aerobic plate count | 霉菌和酵母菌/(CFU·mL-1) mould & yeast | 大肠菌群/(MPN·mL-1) coliform | 食源性致病菌 foodborne pathogen | |
GB 16740 | ≤100 | ≤20 | ≤0.1 | 阴性negative(ND) | |
未灭菌non-sterilized | 4200 | 600 | 28 | 阴性negative(ND) | |
微波灭菌 microwave sterilization | 30 s | 2900 | 500 | 16 | 阴性negative(ND) |
60 s | 1500 | 300 | 15 | 阴性negative(ND) | |
90 s | 600 | 200 | 14 | 阴性negative(ND) | |
煮沸灭菌 boiling sterilization | 15 min | 20 | 60 | 阴性negative(ND) | 阴性negative(ND) |
20 min | <10 | 30 | 阴性negative(ND) | 阴性negative(ND) | |
25 min | <10 | 10 | 阴性negative(ND) | 阴性negative(ND) | |
30 min | ND | ND | 阴性negative(ND) | 阴性negative(ND) | |
高压蒸汽灭菌 high pressure steam sterilization | 121 ℃,15 min | <10 | ND | 阴性negative(ND) | 阴性negative(ND) |
表6
不同灭菌工艺对有效成分含量与抗氧化活性的影响"
灭菌工艺 treatment | RABTS+·/(μmol·g-1) | RFRAP/(μmol·g-1) | IC50, DPPH·/(mg·L-1) | TPC/(μmol·g-1) | TFC/(μmol·g-1) | CAT/(mg·g-1) | FER/(mg·g-1) | HYP/(mg·g-1) | RUT/(mg·g-1) | QUE/(mg·g-1) | AFZ/(mg·g-1) |
未灭菌 non-sterilization | 2.17±0.032 | 1.26± 0.006 | 343.94±1.23 | 0.0148 | 0.0203 | 30.03± 0.78 | 14.12±0.47 | 68.42± 0.56 | 20.31±0.39 | 63.21± 0.52 | 17.21±0.34 |
高压蒸汽灭菌 high pressure steam sterilization | 2.06±0.028 | 1.2± 0.008 | 477.88±2.24 | 0.0138 | 0.019 | 28.21± 0.66 | 13.21±0.37 | 67.22± 0.54 | 19.57±0.52 | 61.21± 0.46 | 16.73±0.35 |
煮沸灭菌 boiling sterilization | 2.09±0.031 | 1.21± 0.005 | 436.48±1.35 | 0.0141 | 0.0198 | 28.76± 0.71 | 13.72±0.51 | 65.32± 0.64 | 19.85±0.48 | 62.76± 0.42 | 16.78±0.28 |
表7
化学稳定性试验中该饮料的活性成分含量及抗氧化活性"
化学稳定性试验 chemical stability test | 天数/d day | TPC/(μmol·g-1) | TFC/(μmol·g-1) | RABTS+·/(μmol·g-1) | RFRAP/(μmol·g-1) | CAT/(mg·g-1) | FER/(mg·g-1) | HYP/(mg·g-1) | RUT/(mg·g-1) | QUE/(mg·g-1) | AFZ/(mg·g-1) |
高温试验 high temperature assays | 0 | 0.0141 | 0.0198 | 2.09±0.01 | 1.21± 0.03 | 28.76±0.20 | 13.72± 0.16 | 65.32±0.55 | 19.85± 0.27 | 62.76±0.36 | 16.78± 0.22 |
5 | 0.0137 | 0.0194 | 2.04±0.02 | 1.19± 0.02 | 27.96±0.51 | 13.52± 0.44 | 63.89±0.55 | 19.12± 0.62 | 61.52±0.39 | 16.22± 0.33 | |
10 | 0.0134 | 0.019 | 2.00±0.02 | 1.18± 0.03 | 27.48±0.42 | 13.35± 0.52 | 62.24±0.35 | 19.02± 0.47 | 60.78±0.26 | 16.08± 0.35 | |
强光试验 strong illu mination assays | 5 | 0.0138 | 0.0196 | 2.05±0.04 | 1.19± 0.05 | 28.52±0.54 | 13.48± 0.27 | 64.3±0.37 | 19.58± 0.25 | 62.05±0.61 | 16.34± 0.24 |
10 | 0.0136 | 0.019 | 2.02±0.04 | 1.17± 0.05 | 27.89±0.43 | 13.22± 0.52 | 62.31±0.36 | 19.23± 0.24 | 61.57±0.24 | 16.16± 0.12 | |
加速试验 accelerated tests | 30 | 0.014 | 0.0196 | 2.07±0.07 | 1.20± 0.04 | 28.40±0.57 | 13.64± 0.52 | 63.69±0.44 | 19.83± 0.34 | 62.18±0.31 | 16.68± 0.33 |
60 | 0.0138 | 0.0194 | 2.03±0.02 | 1.18± 0.02 | 28.38±0.53 | 13.50± 0.27 | 63.76±0.34 | 19.47± 0.25 | 62.16±0.24 | 16.39± 0.32 | |
90 | 0.0137 | 0.0194 | 2.02±0.05 | 1.17± 0.06 | 27.19±0.45 | 13.43± 0.47 | 62.86±0.34 | 19.31± 0.31 | 61.07±0.41 | 16.35± 0.30 | |
180 | 0.0135 | 0.019 | 1.99±0.04 | 1.16± 0.02 | 27.38±0.33 | 13.15± 0.37 | 62.90±0.34 | 19.02± 0.47 | 60.86±0.24 | 16.11± 0.29 |
表8
保质期验证试验中该饮料的活性成分含量及抗氧化活性"
天数/d day | TPC/(μmol·g-1) | TFC/(μmol·g-1) | RABTS+·/(μmol·g-1) | RFRAP/(μmol·g-1) | CAT/(mg·g-1) | FER/(mg·g-1) | HYP/(mg·g-1) | RUT/(mg·g-1) | QUE/(mg·g-1) | AFZ/(mg·g-1) |
0 | 0.0141 | 0.0198 | 2.09±0.01 | 1.21± 0.03 | 28.76±0.20 | 13.72± 0.16 | 65.32±0.55 | 19.85± 0.27 | 62.76±0.36 | 16.78± 0.22 |
90 | 0.0139 | 0.0194 | 2.04±0.03 | 1.19± 0.04 | 27.79±0.36 | 13.35± 0.25 | 63.71±0.54 | 19.19± 0.22 | 60.68±0.18 | 16.32± 0.11 |
180 | 0.0135 | 0.0190 | 2.00±0.01 | 1.17± 0.04 | 28.11±0.18 | 13.27± 0.25 | 62.20±0.64 | 19.22± 0.16 | 60.79±0.33 | 16.38± 0.21 |
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