5 8 Vol. 5 No. 8 2014 8 Journal of Food Safety and Quality Aug., 2014 陈智毅 1*, 刘学铭 1, 杨春英 1, 杨荣玲 1, 王思远 1, 唐秋实 1, 林耀盛 1, 唐选明 (1., 510610; 2., 100193) 2 摘要 : 目的 CO 2 方法 CO 2,, - 结果,, 15 MPa 55 1.5 h,, 52.00% 1.07% 11, (40.26%)(29.27%) (16.12%)(7.38%) 结论, 关键词 : ; (Zophobas morio); The supercritical carbon dioxide extraction of superworm oils and analysis by gas chromatograph-mass spectrometry CHEN Zhi-Yi 1*, LIU Xue-Ming 1, YANG Chun-Ying 1, YANG Rong-Ling 1, WANG Si-Yuan 1, TANG Qiu-Shi 1, LIN Yao-Sheng 1, TANG Xuan-Ming 2 (1. Sericultural and Agri-Food Research Institute, Guangdong Academy of Agricultural Sciences, Guangzhou 510610, China; 2. Key Laboratory of Agro-Products Processing, Ministry of Agriculture, Institute of Agro-Products Processing Science and Technology CAAS, Beijing 100193, China ABSTRACT: Objective Study on supercritical carbon dioxide (SC-CO 2 ) extraction technology and fatty acid composition of superworm (Zophobas morio) fed by Flammulina velutipes bran. Methods The effects of extraction pressure and temperature on the extraction rate of superworm oil which was extracted by supercritical CO 2 were discussed, and the fatty acid composition of superworm oil after methyl esterification was analyzed by gas chromatography-mass spectrometry (GC-MS). Results The order of superworm oil extraction factors was extraction pressure>temperature>time. Consider the cost of production, this experiment selected the condition of 15 MPa, 55, 1.5 h, under the condition, the extraction rate was 52.00%±1.07%. 11 kinds of fatty acids from superworm oil by gas chromatograph-mass spectrometry were identified, mainly oleic acid (40.26%), pal- 基金项目 : ( ) (201303080) (2011A011303002 2012B091100468 2012A020100008) Fund: Supported by Special Fund for Agro-scientific Research in the Public Interest (201303080) and Guangdong Province Science and Technology Plan Project (2011A011303002, 2012B091100468, 2012A020100008) * 通讯作者 :,,, E-mail: fezychen@scut.edu.cn *Corresponding author: CHEN Zhi-Yi, Associate Professor, Sericultural and Agri-Food Research Institute, Guangdong Academy of Agricultural Sciences, No.133, Yihenglu Dongguangzhuang, Tianhe District, Guangzhou 510610, China. E-mail: fezychen@scut.edu.cn
8, : 2533 mitic acid (29.27%), linoleic acid (16.12%), and stearic acid (7.38%), etc. Conclusion Superworm oil has high edible and medicinal value, which enables waste and agricultural by-products to be turned into superworm by biotransformation technology, and supplies oil resources of food, feed and renewable energy continuously. KEY WORDS: supercritical carbon dioxide extraction; superworm(zophobas morio) oil; gas chromatograph-mass spectrometry 1 引言 (Zophobas morio),, 51%, 29%,,,,, [1-3], [4],, [5] CO 2 (supercritical carbon dioxide, SC-CO 2 ) [6-7] CO 2,, CO 2 [8-12] SC-CO 2,, SC-CO 2 ; (gas chromatograph-mass spectrometry, GC-MS), 2 材料与方法 2.1 材料与仪器, [5] CO 2 (.5%), HL-1L/50MPa-HB ( ); S2C-C ( ); 6890N-5973B - ( Agilent ); JM1000Max1000 ( ); BS-124S (Sartorius ); 202-3 ( ); DG160 ( ); GHRH-20 () 2.2 实验方法 2.2.1 样品前处理,,,, 35 5%,, 2.2.2 超临界 CO 2 萃取大麦虫油脂工艺流程, CO 2 : (%)=( / ) 100% [13, 14] 2.2.3 萃取实验设计 CO 2,,, (A) (B) (C),,,, L 9 (3 3 ),, 1, 9, 3 [15] 2.2.4 油脂成分分析方法 : : 0.5 g, 5 ml0.5 表 1 因素水平表 Table 1 Factor level charts A /MPa B / C /h 1 20 55 2 2 15 45 1.5 3 10 35 1
2534 5 mol/l, 30 min; 5 ml, 2 min, ( 20 ), : Agilent 6890N ; : DB-WAX (30 m 320 μm 0.25 μm); : 250 ; FID : 250 ; : 80, 10 /min 200, 2 /min 230, 1 min; : 20:1; : He, 20 ml/min : (EI) ; 70 ev; 275 ; 200 ; m/z285; 1.5 V; m/z 30~ 450 Nist05a 3 结果与分析 3.1 单因素实验 3.1.1 压力对萃取率的影响 1 55, 1,,, 15 MPa 20 MPa,, 15 MPa, 1 h, 1.5h, 2 h 3.1.2 温度对萃取率的影响 2 20 MPa, 2,,, 55, 1 h, 1.5 h, 2 h 2 Fig. 2 Effects of temperature on extraction rate 3.1.3 时间对萃取率的影响, 1 2,, 1 h, 1.5 h, 2 h,,, 3.2 大麦虫油脂超临界 CO 2 萃取最佳工艺条件的确定 2, Table 2 表 2 正交实验结果及分析 The results of orthogonal experiment and analysis A /MPa B / C /h % 1 20(1) 55(1) 2.0(1) 56.52 2 20(1) 45(2) 1.5(2) 42.96 3 20(1) 35(3) 1.0(3) 31.93 4 15(2) 55(1) 1.5(2) 52.00 5 15(2) 45(2) 1.0(3) 23.69 6 15(2) 35(3) 2.0(1) 37.88 7 10(3) 55(1) 1.0(3) 34.43 8 10(3) 45(2) 2.0(1) 21.95 9 10(3) 35(3) 1.5(2) 12.95 K1 131.41 142.95 116.35 K2 113.57 88.60 107.91 K3 69.33 82.76 90.05 k 1 43.80 47.65 38.78 k 2 37.86 29.53 35.97 k 3 23.11 27.59 30.02 1 Fig. 1 Effects of extraction pressure on superworm oil extraction rate R 20.69 20.06 8.76 20 55 2
8, : 2535 A B C, A 1 B 1 C 1, 20 MPa 55 2 h, 56.52% 2 h,,, 2 h, 2 h,, A 2 B 1 C 2, 15 MPa 55 1.5 h,,, 52.00% 1.07% 3.3 大麦虫油脂气质联用分析图谱 55, 20 MPa, 1 h 1.5 h 2 h GC-MS, 3 3 1 h 1.5 h 2 h, GC-MS,,, 3.4 大麦虫油脂中主要化学成分 GC-MS 分析结果 GC-MS, Nist05a,, 11, 3, 40.26% 29.27% 16.12% 7.38% 4 讨论 CO 2, Fig. 3 3 GCMS GC-MS Chromatogram of superworm oil with different extraction time
2536 5 表 3 大麦虫油脂脂肪肪酸组成 Table 3 Superworm fatty acid composition (% %) 1 methyl tetradecanoate 242 1.41 98 C 15 H 3 30O 2 2 tetradecanoic acid, 12-methyl-, methyl ester 12-270 0.50 92 C 16 H 3 32O 2 3 pentadecanoic acid, methyl ester 256 0.39 98 C 16 H 3 32O 2 4 hexadecanoic acid, methyl ester 270 29.27 92 C 17 H 3 34O 2 5 9,12-hexadecadienoic acid, methyl ester -9,12-266 0.69 C 16 H 3 30O 2 6 9-hexadecenoic acid, methyl ester, (Z)- -9-268 2.82 C 17 H 3 32O 2 7 hexadecanoic acid, 14-methyl-, methyl ester 14-284 0.11 96 C 17 H 3 34O 2 8 heptadecanoic acid, methyl ester 284 0.73 C 18 H 3 36O 2 9 9, 12-octadecadienoic acid, methyl ester -9,12- ( ) 294 16.12 C 19 H 3 34O 2 10 9-octadecenoic acid (Z)-, methyl ester 297 40.26 C 19 H 3 36O 2 11 octadecanoic acid, methyl ester ( ) 298 7.38 98 C 19 H 3 38O 2 20 MPa 55 2.0 h, 56.52%, 48.% 15.37% [6],,,
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