Optimization of Ultrasound-Assisted Extraction of Cornus officinalis Seed Oil by Response Surface Methodology and Chemical Composition Analysis

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1 2012, Vol., No * ( 7062) (RSM) 40 40min :1(mL/g) 97.08%( 7.90%) GC-MS (61.89%) (19.99%) (7.6%) (6.%) 69.45% VE 76.0mg/0g (RSM) Optimization of Ultrasound-Assisted Extraction of Cornus officinalis Seed Oil by Response Surface Methodology and Chemical Composition Analysis LIU Rui-lin ZHAN Han-ying CHEN Tian MOU Zhao-li JIA Xiao-meng ZHANG Zhi-qi* (Key Laboratory of Medicinal Resource and Natural Pharmaceutical Chemistry, Ministry of Education, School of Chemistry and Chemical Engineering, Shaanxi Normal University, Xi an 7062, China) Abstract Response surface methdology was employed to optimize the ultrasound-assisted extraction of Cornus officinalis seed oil. Meanwhile, its chemical composition was analyzed by GC-MS. The optimal extraction conditions were determined as 40 of extracion temperatrure, 40 min of extraction time, and :1 of liquid-to-solid raio (ml/g). Under these conditions, the extraction yield of Cornus officinalis seed oil based on the dry weight of Cornus officinalis kernels was 7.90%, accounting for 97.08% of that obtained from Soxhlet extraction. The predominant fatty acids in Cornus officinalis seed oil were oleic acid (61.89%), stearic acid (19.99%), palmitic acid (7.6%), linoleic acids (6.%), and so on. The percentage of unsaturated fatty acids relative to total fatty acids was 69.45%. In addition, the vitamin E content in Cornus officinalis seed oil, as determined by HPLC, was 76.0 mg/0 g. Key words Cornus officinalis seed oil ultrasound-assisted extraction chemical composition analysis response surface methodology (RSM) TS224.4 A (2012) (Cornus officinalis Sieb. et Zucc.) [4-6] [1] [2] [ ] (208760) 2012 (1987 ) liuruilin2009@stu.snnu.edu.cn * ( ) zqzhang@snnu.edu.cn

2 2 2012, Vol., No. 12 [7] 0min [8-] (response surface methodology = 0 RSM) [11-14] /%= 0 (gas chromatography-mass spectrometry GC-MS) (high performance liquid chromatography HPLC) VE 1. (6:1 8:1 :1 12:1 14:1(mL/g)) ( ) ( ( 0.%) VE ( 98% ) ( ) Honeywell Box-Behnken ( 2) (Y) FW 400A Y 0 i Xi ii Xi 2 ijxixj i=1 i=1 i=1 j=i+1 Y X i X j RE-52A ZK- 0 i ij 82A QP20 i i - LC-A TGL-16C Millipore g min) (X 1) (X2) (X) X1 (ml/g) X2 / mL 2mL 5.0g 0.5mol/L KOH 1 1mL 2mL 15 20min 2mol/L 55 15min 1 6h 1 0 m L GC-MS Table 1 Variables and levels of Box-Behnken design X /min [15] -

3 2012, Vol., No. 12 RTX-5 MS 5% diphenyl-95% dimethyl polysiloxane (0m 0.25mm 0.25 m) :1mL/g 99.8kPa (99.999%) 1.46mL/min 20: /min 220 2min /min L (electron impact EI) eV 0.9 kv 4 mi n u LCsolution NISTNIST27 NIST VE g mL 60% KOH 6g 15mL 0min 0mL 0 0 ml 4 Na 2SO ml H P L C Agilent HC-C18 (4.6mm 2mm 5 m) : (98:2 V/V) 0.8mL/min 1 0 L n m W [16-17] 2 00 W W W 0min :1(mL/g) :1(mL/g) / 2 Fig.2 Effect of extraction temperature on Cornus officinalis seed oil yield :1mL/g :1 8:1 :1 12:1 14:1 (ml/g) 1 Fig.1 Effect of ratio of liquid to solid on Cornus officinalis seed oil yield /min Fig. Effect of extraction time on Cornus officinalis seed oil yield

4 4 2012, Vol., No X 2 (P 0.05) X 1 X 1 2 X 2 2 (P 0.01) 45min 45min Box-Behnken (BBD) 15 2 Design-Expert software 7.1. Trial (State-Ease Inc., Minneapolis, MN, USA) Y X X2 2.2X X1X X1X 0.015X2X 0.842X X X 2 2 BBD Table 2 Box-Behnken design arrangement and corresponding seed oil yield X1 X2 X Y (ml/g) / /min /% 1 1(4) 1(0) 0(45) (12) () (40) 1(0) (60) (8) P F P ** X ** X X * X1X X1X X2X X ** X ** X * F 1.4 F0.05(9,2) 19.8 F C 5 45 F0.05(9,2) 8.81 P min RSM Table Analysis of variance (ANOVA) for the fitted quadratic polynomial model *.P 0.05 **.P % R R 2 Adj (CV).% A 0min :1(mL/g) 4A :1 :1(mL/g) 40 4B 8:1 :1(mL/g) min 8:1(mL/g) 4C 5A / ( 5B) R 2 Adj % X

5 2012, Vol., No min 9.61:1(mL/g) 97.9% 40 40min :1(mL/g) 97.08% ( 7.90%) 1% X/min A. X/min C. 4 Fig.4 Response surface and contour plots for the interative effects of three extraction parameters on Cornus officinalis seed oil yield /% 99 A X/min B X/min (A) (B) Fig.5 Standardized residual plot (A) and fitted curve for predicted versus experimental values (B) of Cornus officinalis seed oil yield B. 2. GC-MS ( 6)

6 6 2012, Vol., No. 12 ( 4) % (61.89%) (6.%) % (19.99%) (7.6%) /% /min 6 GC-MS Fig.6 GC-MS total ion chromatogram of fatty acid methyl esters of Cornus officinalis seed oil 4 Table 4 Fatty acid composition of Cornus officinalis seed oil mau HPLC E VE HPLC 7(A) 7(B) VE( - ) y 2960x 462 R mg/mL VE 76.0mg/0g VE [18-19] B 7 VE (A) (B)HPLC Fig.7 HPLC chromatograms of vitamin E standard (A) and vitamin E VE /min in Cornus officinalis seed oil (B) /min /%.27 C12H24O C14H28O C16H0O C16H2O C16H0O C17H4O C18H4O C18H6O , -12-C18H2O ,8,11,14-C20H2O C20H8O ,11-C20H6O C20H40O C20H44O C24H46O C24H48O VE mau A /min VE 97.08% ( 7.90%) [20] VE [1]. : [S]. :, 20: 26. [2]. [J]., 1990, 12(12): 46. []. [J]., 1990, 15(1): [4],,. [J]., 2001, (11): [5],,. [J]., 1995, 26 (2): [6] DU Weifeng, CAI Hao, WANG Mingyan, et al. Simultaneous determination of six active components in crude and processed Fructus Corni by high performance liquid chromatography[j]. Journal of Pharmaceutical and Biomedical Analysis, 2008, 48(1): [7],,,. [J]., 2004(9):

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