6 6 Vol. 6 No. 6 2015 6 Journal of Food Safety and Quality Jun., 2015 黄俊魏, 唐琳 *, 陈浩 (, 250014) 摘要 : 目的,, 方法, ph, -, 结果 : 130 W, 20 min, 4:30(g/mL), 50%, (0.22±0.02) mg/g, (0.83±0.02) mg/g (0.74±0.02)mg/g 结论, 关键词 : ; ; Optimization of technology for ultrasound-assisted sequential extraction of rose essential oil and pigment HUANG Jun-Wei, TANG Lin *, CHEN Hao (Department of Food Science and Engineering, College of Life Science, Shandong Normal University, Jinan 250014, China) ABSTRACT: Objective To optimize the fractionation extraction of rose essential oil and pigment from Pingyin rose by ultrasound technology, not only extracted rose essential oil but also increased the yield of pigment. Methods Pingyin rose petals was used as raw material, the rose essential oil and pigments were extracted by ultrasonic-assisted ethanol aqueous. The rough yield of rose pigment was measured by ph-differential method, and the gas chromatography was used to determine the relative content of essential oils. The ether-petroleum ether mixture was used to extract rose essential oil, and macroporous resin was used in the purification of pigment. Results The optimized best extraction parameters: ultrasonic-assisted extraction time 20 min, ultrasound power 130 W, liquid-solid ratio 4:30 (g/ml), ethanol concentration 50%, then the yield of rose essential oil (0.22±0.02) mg/g, and crude yield of pigment (0.83±0.02) mg/g. The purified yield of pigment (0.74±0.02) mg/g. Conclusion Rose essential oil are extracted using ultrasonic technology, and the high yield of the pigment are achieved. KEY WORDS: ultrasound; rose essential oil; rose pigment extraction 1 引言,, [1],, [2], [3], * 通讯作者 :,, E-mail: tanglin@sdnu.edu.cn *Corresponding author: TANG Lin, Associate Professor, Natural Functional Products, Department of Food Science and Engineering, College of Life Science, Shandong Normal University, Jinan 250014, China. E-mail: tanglin@sdnu.edu.cn
2124 6, [4,5],,,,,,, [3],,, [6], ; ;,, [7], [8] -3-,,,, [9-11], [12],,,, [13],,, ( 1),,, 2 材料与方法 2.1 材料 试剂与仪器 : (, 5 ) : (, ); (, ); (, ); (, ); (, ); (, ); ( 30 60, ); (, ) Fig. 1 1 The process route of ultrasound sequential extraction : UV-1700 ( ); JY92-Ⅱ ( ); DK-450B ( ); (centrifuge 5810 R); AR1530( - ); DV214( ); GC-2014 ( ) 2.2 玫瑰精油和色素提取的工艺优化 2.2.1 超声前处理, 30 ml,,, 6000 r/min 10 min, 2.2.2 玫瑰精油相对含量的测定 8 ml, 10 ml, 1 μl, 1 ml [14]
6, : 2125, 5 min, 6000 r/min 1 min, 1.5 ml, 4, 1 μl,, : KB-5 (30 m 0.32 mm, 0.25 μm), (FID); : 50 220, 3 /min, 220 10 min; (N 2 ) 0.5 ml/min; 1 μl, 1:5; : 4 min, 250, 250 2.2.3 色素含量的测定 ph [15], 0.25 ml, ph 1.0 ph 4.5 3 ml, 13, 40 20 min [16],, 520 nm 700 nm, - A= bc, Fuleki [17], 2.2.4 ph 示差法 (1) [18] ph 1.0 : 1.86 g, 980 ml, ph 1.0, 1000 ml ph 4.5 : 54.43 g, 960 ml, ph 4.5, 1000 ml (2) [17] A=(A 520 nm -A 700 nm ) ph1.0 -(A 520 nm -A 700 nm ) ph4.5 A Mw DF C (1) L 1000 C V (mg/g) = 1000 (2) M (1) : A ; Mw -3- ( 449.2); DF ; -3- ( 26900 L/(mol cm)); L (1 cm) (2) : C (g/ml); V (ml); M (g) 2.2.5 单因素试验 ph [19],,, ;,,, ph 3 (1) 5.0 g, 30 ml 40%, 15 min, (650 W) 10% 15% 20% 25% 30% (2) 5.0 g, 30 ml, 25%, 15 min, 30% 40% 50% 60% 70% (3) 5.0 g, 30 ml 40%, 25%, 10 min 15 min 20 min 25 min 30 min (4) 2.0 g 3.0 g 4.0 g 5.0 g 6.0 g, 30 ml 40%, 25%, 25 min, 2.2.6 正交试验,, L 16 (4 5 ), 1,, 2.3 玫瑰精油的提取, 4g, 3, 6000 r/min 10 min,, 20 ml 1:2 [21], 3,, 55,,,
2126 6 2.4 色素的提取及纯化, 0.25 ml, ph=2.0 7 20 g AB-8 (1 cm 35 cm), 7.2 BV/h(BV ),, 10 ml, 10% ( ),,,, ph=1 70%, 2.7 BV/h,,, [22] 3 结果与讨论 3.1 气相色谱图 2, 5.58 min,, 56.81 min,, [20],, ( ),, 3.2 各单因素最优条件的确定 3.2.1 超声功率的确定 5.0 g, 30 ml 40%, 15 min, 3 3,,,,,, 20%(650 W), 130 W, ; 25%(650 W), 162.5 W,,,,,, Table 1 表 1 因素水平表 Factors and levels of orthogonal experiment A (min) B (650 W) C (g/30 ml) D 1 15 15% 3 30% 2 20 20% 4 40% 3 25 25% 5 50% 4 30 30% 6 60% Fig. 2 2 The gas chromatograph of Pingyin rose essential oil
6, : 2127, 25%,, 5 Fig. 3 3 Effect of ultrasonic power on the extraction 3.2.2 乙醇浓度的确定 5.0 g, 30 ml, 25%, 15 min, 4 Fig. 4 4 Effect of ethanol concentration on the extraction 5 Fig. 5 Effect of ultrasonic time on the extraction 5,,, 20 min, ; 25 min,,, ;, 3.2.4 料液比的确定, 30 ml 40%, 25%, 25 min,, 6 4,,,,,,, 40%,, ; 50%,,,, 3.2.3 超声时间的确定 5.0 g, 30 ml 40% Fig. 6 6 Effect of solid-liquid ratio on the extraction
2128 6 6,,,,, 4:30(g/mL) ; 5:30(g/mL),,, 3.3 正交试验结果及分析, 1, 2 2,, C( )>D( )>B( )>A( ), Table 2 表 2 正交试验结果 Orthogonal experimental data and results A B C D (mg/g) (10-2 ) 1 1 1 1 1 0.69 4.17 2 1 2 2 2 0.95 5.74 3 1 3 3 3 0.83 5.62 4 1 4 4 4 0.82 4.33 5 2 1 2 3 0.86 5.85 6 2 2 1 4 0.74 5.53 7 2 3 4 1 0.91 4.76 8 2 4 3 2 1.02 5.24 9 3 1 3 4 0.81 4.73 10 3 2 4 3 0.86 5.28 11 3 3 1 2 0.90 5.09 12 3 4 2 1 0.85 4.53 13 4 1 4 2 0.82 4.39 14 4 2 3 1 0.76 4.82 15 4 3 2 4 0.94 4.45 16 4 4 1 3 0.72 4.21 K 0.822 0.795 0.762 0.802 K 0.883 0.827 0.900 0.922 K 0.855 0.895 0.855 0.817 K 0.810 0.853 0.852 0.828 K 4.965 4.785 4.750 4.570 K 5.345 5.343 5.143 5.115 K 4.908 4.980 5.103 5.240 K 4.468 4.578 4.690 4.760 R 0.073 0.100 0.138 0.120 R 0.877 0.765 0.453 0.670
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