Optimized Extraction of Functional Ingredients from Callicarpa nudiflora Hook.et Arn.by Box-Behnken Design
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摘要: 为研究裸花紫珠浸膏得率、总黄酮、总酚酸及总皂苷的最佳提取工艺，以浸膏得率和有效成分总含量（总黄酮、总酚酸及总皂苷含量之和）的加权评分值（加权评分值=浸膏得率×0.7+总有效成分含量×0.3）为指标，通过单因素和响应面设计相结合的方法，以提取方法、提取时间、料液比、乙醇浓度、提取次数为考察因素，优化裸花紫珠有效成分提取工艺。结果表明裸花紫珠有效成分的最佳提取工艺为：超声提取时间为42 min，料液比1：17，乙醇体积分数为62%，提取2次。此条件下加权评分值为119.27，预测加权评分值为120.47，两者相差较小。优化后的裸花紫珠有效成分提取工艺简单可行，重现性和可预测性较好。Abstract: To optimize the extraction of functional ingredients from the leaves of Callicarpa nudiflora Hook. et Arn., an experiment based on the Box-Behnken design was conducted. The extraction rate and contents of functional ingredients including flavonoids, phenolic acids, and saponins in the resulting extracts were weighed against the method, duration, cycle, material to solvent ratio, and ethanol concentration of the process. The weighted value for evaluation was calculated by the formula of(dry weight extract 0.7+ combined weight of functional ingredients 0.3). The optimized conditions included the application of ultrasound for 42 min, a material:solvent ratio of 1:17, the use of 62% ethanol for solvent, and two extraction cycles to arrive at a weighted value of 119.27, which was close to the predicted value of 120.47. The established extraction process was simple and applicable with desirable reproducibility and predictability.
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图 2 响应面图与等高线叠加
Figure 2. Response surface diagram and contour line superposition diagram
表 1 Box-Behnken设计试验水平及因素
Table 1. Levels and factors of Box-Behnken experimental design
因素 水平 -1 0 1 提取时间/min 30 40 50 料液比/(g·mL-1) 1:10 1:15 1:20 乙醇体积分数/% 45 60 75 
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表 2 不同提取方法对裸花紫珠有效成分提取率的影响
Table 2. Effects of different extraction methods on the functional ingredients extraction rates of Callicarpa nudiflora
提取方法 浸膏得率/% 总黄酮/(mg·g-1) 总酚酸/(mg·g-1) 总皂苷/(mg·g-1) 有效成分总含量/(mg·g-1) 煎煮 14.30e 57.21b 23.56b 24.27bc 105.05cd 回流 19.00b 78.16a 33.73a 23.60bc 135.49b 水浴 17.10c 62.24b 22.71b 28.45ab 113.38c 超声水提 14.90d 49.42c 22.04b 23.27c 94.72d 超声醇提 24.70a 83.14a 33.40a 31.72a 148.25a 注：多重比较采用Duncan′s法，各成分同列中不同小写字母表示差异显著(P < 0.05)。
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表 3 中心组合试验设计与结果
Table 3. Design and results of central combination experiment
试验编号 提取时间/min 料液比(1:x) 乙醇体积分数/% 总黄酮/(mg·g-1) 总酚酸/(mg·g-1) 总皂苷/(mg·g-1) 浸膏得率/% 总有效成分/(mg·g-1) 加权评分值 1 30 10 60 108.52 48.27 55.58 24.80 212.37 81.07 2 50 10 60 107.50 45.54 57.91 25.60 210.94 81.20 3 30 20 60 148.46 67.19 66.35 28.00 282.00 104.20 4 50 20 60 154.85 61.04 79.14 29.40 295.04 109.09 5 30 15 45 147.39 43.90 59.77 26.20 251.06 93.66 6 50 15 45 161.86 46.53 93.52 27.00 301.91 109.47 7 30 15 75 168.55 57.81 61.79 28.40 288.15 106.32 8 50 15 75 162.97 53.03 62.21 27.60 278.21 102.78 9 40 10 45 109.25 35.57 59.10 23.60 203.92 77.70 10 40 20 45 161.11 50.87 54.96 28.60 266.94 100.10 11 40 10 75 126.45 51.12 60.42 25.80 237.99 89.46 12 40 20 75 163.46 55.06 66.45 29.80 284.97 106.35 13 40 15 60 156.67 66.50 69.66 29.20 292.83 108.29 14 40 15 60 159.93 64.23 75.39 29.80 299.55 110.73 15 40 15 60 160.08 67.70 76.79 29.40 304.57 111.95 16 40 15 60 160.98 59.42 92.56 30.00 312.95 114.89 17 40 15 60 183.55 68.07 71.01 30.20 322.63 117.93
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表 4 响应面二次回归方程方差分析
Table 4. Analysis of variance for response quadratic regression equation
来源 自由度 均方 离差平方和 F P 模型 9 263.6762 2373.0857 18.8611 0.0004 A-提取时间 1 37.3828 37.3828 2.6740 0.1460 B-料液比 1 1019.6881 1019.6881 72.9396 < 0.0001 C-体积分数 1 71.9308 71.9308 5.1453 0.0576 AB 1 5.6628 5.6628 0.4051 0.5447 AC 1 93.6654 93.6654 6.7000 0.0360 BC 1 7.5887 7.5887 0.5428 0.4852 A2 1 89.2273 89.2273 6.3825 0.0394 B2 1 856.3946 856.3946 61.2590 0.0001 C2 1 109.2284 109.2284 7.8133 0.0267 残差 7 13.9799 97.8592 失拟项 3 13.9458 41.8373 0.9957 0.4804 纯误差 4 14.0055 56.0219 总和 16 2470.9450
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