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1 6 6 Vol. 6 No Journal of Food Safety and Quality Jun., 2015 黄俊魏, 唐琳 *, 陈浩 (, ) 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 , 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 :,, 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 , China. tanglin@sdnu.edu.cn

2 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超声前处理, 30 ml,,, 6000 r/min 10 min, 玫瑰精油相对含量的测定 8 ml, 10 ml, 1 μl, 1 ml [14]

3 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); : , 3 /min, min; (N 2 ) 0.5 ml/min; 1 μl, 1:5; : 4 min, 250, 色素含量的测定 ph [15], 0.25 ml, ph 1.0 ph ml, 13, min [16],, 520 nm 700 nm, - A= bc, Fuleki [17], ph 示差法 (1) [18] ph 1.0 : 1.86 g, 980 ml, ph 1.0, 1000 ml ph 4.5 : 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- ( L/(mol cm)); L (1 cm) (2) : C (g/ml); V (ml); M (g) 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, 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,,,

4 色素的提取及纯化, 0.25 ml, ph= 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,, min,, [20],, ( ),, 3.2 各单因素最优条件的确定超声功率的确定 5.0 g, 30 ml 40%, 15 min, 3 3,,,,,, 20%(650 W), 130 W, ; 25%(650 W), 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 % 3 30% % 4 40% % 5 50% % 6 60% Fig. 2 2 The gas chromatograph of Pingyin rose essential oil

5 6, : 2127, 25%,, 5 Fig. 3 3 Effect of ultrasonic power on the extraction 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,,, ;, 料液比的确定, 30 ml 40%, 25%, 25 min,, 6 4,,,,,,, 40%,, ; 50%,,,, 超声时间的确定 5.0 g, 30 ml 40% Fig. 6 6 Effect of solid-liquid ratio on the extraction

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 ) K K K K K K K K R R

7 6, : 2129 C 2 D 2 B 3 A 2, 4:30 (g/ml), 40%, 20 min, 25%(650W); A( )>B( )>D( )>C( ), A 2 B 2 D 3 C 2, 20 min, 20%(650 W), 50%, 4:30(g/mL),,,,,,,,,,,, 20 min, 20%(650 W), 50%, 4:30(g/mL) 3.4 玫瑰精油的提取及色素的分离纯化结果, 3,,, (0.22±0.02) mg/g; ph (0.83±0.02) mg/g, AB-8, 90%, 99%, (0.74±0.02) mg/g 4 结论,,,,, 4,, : 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 参考文献 [1]. [D]. :, Mou ZH. Determination of proanthocyanins and study on the quality standard in rosa rugosa of Shandong province [D]. Jinan: Shandong University of Traditional Chinese Medicine, [2]. [D]. :, Li ZJ. Study of the extraction process and properties of anthocyanin from Pingyin roses [D]. Jinan: Shandong Normal University, [3],,,. [J] , 11: Hu XY, Shen CH, Ao ZH, et al. Research progress in the active ingredients of rose and rose wine [J]. Liquor-making Sci Technol, 2014, 11: [4]. CO 2 [D]. : Xie QT. Research on optimization of processing parameters for supercritical carbon dioxide extraction of rose essential oil and comprehensive utilization of by products [D]. Changsha: Central South University, [5],. [J] , 29(196): Jia JJ, Miao MS. Analysis of chemistry, pharmacology and clinical application for rose [J]. China J Chin Med, 2014, 29(196): [6],,. [J]., 2006, 27(3): Chen W, Meng XJ, Wang LN. Studies on the extraction technology of red pigment from rose [J]. Food Res Dev, 2006, 27 (3): [7],,,. [J] , 19(4): Ma XH, Wang YH, Hu YY, et al. Advances in the research of oil-bearing roses [J]. J Northwest For Univ, 2004, 19(4): [8],,,. [J]., 2006, (10): Feng ZS, Du J, Li Y, et al. Purification and preliminary components identification of rose pigment [J]. Food Sci Technol, 2006, (10): [9]. [D]. :, Ying LY. The research of chemical components and functions of essential oil of Rosa damascene [D]. Hangzhou: Zhejiang

8 University, [10],,,. [J]., 2009, 11(11): Wang BX, Peng XQ, Qiao W, et al. Study on assay of anthocyanins in flowers of rose rugosa Thunb [J]. Food Drug, 2009, 11(11): [11],. [J]., 2006, 22(6): Xu YJ, Du QZ. Review on anthocyanins bioactivities [J]. Food Mach, 2006, 22(6): [12]. [D]. :, Zhou XS. Ku-shui rose essential oil and rose residue pigment extraction and purification [D]. Lanzhou: Gansu Agricultural University, [13],,,. [J]., 2015, 16(1): Wang XH, Sun WW, Ji XY. Review on extraction of essential oil from Rosmarinus officialis [J]. J Shanxi Coll Tradit Chin Med, 2015, 16(1): [14] Jannat M, Rold an-guti errez J. Ruiz-Jim enez MD, et al. Ultrasound-assisted dynamic extraction of valuable compounds from aromatic plants and flowers as compared with steam distillation and superheated liquid extraction [J]. Talanta, 2008, (75): [15],,,. ph [J]., 2009, 18: Tang L, Li ZJ, Zhao L, et al. Comparison of Two ph Methods for Determining Anthocyanins from flower petals of rose [J]. Food Sci, 2009, 18: [16],,,. ph [J]., 2011, 11: Sun JC, Liu YT, Zhao YP, et al. Optimization of analytical condition of deter-mining anthocyanins content in blueberry wine by ph-differential method [J]. China Brewing, 2011, 11: [17] Fuleki T, Francis FJ. Quantitative method for anthocyanins: 2.determination of total anthocyanin and degradation index for cranberry juice [J]. Food Sci, 1968, 33(1): [18],,,. ph 73 [J]., 2009, 34(4): , 117. Liu HH, Zhang XL, Du P, et al. Determination the anthocyanin content in Yan73 grape by ph-differential method [J]. China Condiment, 2009, 34(4): , 117. [19],. [J]., 2012, (14): Ge Q, Ma XJ. Study on the extraction and stability of anthocyanins from edible rose [J]. Food Sci Technol Ind, 2012, (14): [20],,,. [J]., 1991, 3(3): Wu QX, Zhang J, Fu DZ, et al. Study on the constituents of essential oil of Pingyin roses [J]. Chin J Chromatogr, 1991, 3(3): [21],,,. [J]., 2014, 42(12): Yang YY, Wang XG, Yang PK, et al. Optimization of technology for ultrasound-assisted extraction of rose essential oil [J]. Jiangsu Agric Sci, 2014, 42(12): [22]. [D]. :, Zhao L. Study of the purification process optimization, molecular modification and application of anthocyanin from Pingyin roses [D]. Jinan: Shandong Normal University, 作者简介 ( 责任编辑 : 白洪健 ) 黄俊魏, 硕士研究生, 主要研究方向为天然功能性成分 @163.com 唐琳, 副教授, 主要研究方向为天然功能性产物 tanglin@sdnu.edu.cn

H 2 SO ml ml 1. 0 ml C 4. 0 ml - 30 min 490 nm 0 ~ 100 μg /ml Zhao = VρN 100% 1 m V ml ρ g

H 2 SO ml ml 1. 0 ml C 4. 0 ml - 30 min 490 nm 0 ~ 100 μg /ml Zhao = VρN 100% 1 m V ml ρ g 16 6 2018 11 Chinese Journal of Bioprocess Engineering Vol. 16 No. 6 Nov. 2018 doi 10. 3969 /j. issn. 1672-3678. 2018. 06. 004 1 2 1 1 1. 330200 2. 330006 4 Box-Behnken 1 25 g /ml 121 92 min 2 6. 284%