7 8 Vol. 7 No. 8 2016 8 Journal of Food Safety and Quality Aug., 2016 张喜金 *, 魏鲜娥, 苏昭仑, 蔡伟江 (, 519040) 摘要 : 目的 方法 -,, 结果, 0.9997 0.9999, 96.8% 101.3%, 0.4 1.0% 结论 β-, β-, 关键词 : ; ; ; ; Determination of the composition and content of phytosterols in wheat germ oil, soybean oil and garlic oil by gas chromatography ZHANG Xi-Jin *, WEI Xian-E, SU Zhao-Lun, CAI Wei-Jiang (By-Health Co., Ltd., Zhuhai 519040, China) ABSTRACT: Objective To establish a method for the determination of the composition and content of phytosterols in wheat germ oil, soybean oil and garlic oil by gas chromatography. Methods Samples were saponified by potassium hydroxide ethanol-methyl tertiary butyl ether solution on water bath, and extracted with iso-octane. Phytosterols were separated by capillary gas chromatography. Results Phytosterols components showed a good linear relationship in the corresponding concentration range, correlation coefficients were from 0.9997 to 0.9999, the average recoveries were 96.8%~101.3%, and the relative standard deviations were between 0.4%~1.0%. Conclusion The phytosterols from wheat germ oil, soybean oil and garlic oil are mainly composed by campesterol, stigmasterol and β-sitosterol, and the highest content is β-sitosterol, the total amount of phytosterols in wheat germ oil is the highest. KEY WORDS: phytosterol; gas chromatography; wheat germ oil; soybean oil; garlic oil 1 引言,, [1-5] ( 1) 4-4- 4,4-3, β-,, C-4 C-11, * 通讯作者 :, E-mail: 215865748@qq.com *Corresponding author: ZHANG Xi-Jin, By-Health Co., Ltd., Zhuhai 519040, China E-mail: 215865748@qq.com
8, : 3389 [6-11] :,, [12], ; [13] ;, [14] ;, [15],,,, ( ), (CNW), ( ), ( ), ( ) 2.3 色谱条件 : 300 ; 10:1; 1 μl: Agilent DB1701(30 m 250 μm 0.25 μm); 4 ml/min : 100 2 min, 20 /min 270, 200 min FID: 300 ; 30 ml/min; 400 ml/min; 30 ml/min 2.4 内标溶液的制备 β- 30.25 mg 25 ml,,, 2.5 对照品溶液的制备 8.75 mg 13.13 mg 12.75 mg β- 30.35 mg 50 ml,, 1.0 2.0 4.0 8.0 16.0 ml 25 ml, 2 ml 2.4 β-,, 2.6 样品溶液的制备 0.5 g 25 ml, 2 ml β-, 4 ml -( 14g 10 ml, 100 ml, 20 ml, ), 80 50 min( 10 min ), 2 ml, 5 ( 10 ml),,,,, 10 ml, 0.45 μm, 3 结果与讨论 1 Fig. 1 Structural formula of phytosterols 2 材料与方法 2.1 实验仪器 7890A ( Agilent ), XP-205 () 2.2 标准与试剂 ( : 99%)( : 99%) ( : 99%) β- ( : 99%) β- ( : 99%) Sigma, 3.1 定性分析与色谱分离,, β- 4 : β- 17.483; 18.294; 19.424; 20.065; β- 21.447 2 3.2 工作曲线的绘制 2.3, GC 1 μl 2.4,,, 1
3390 7 3.3 检出限试验, S/N=3, : 0.15 mg/kg; : 0.44 mg/kg; : 0.19 mg/kg; β- : 0.35 mg/kg 3.4 植物甾醇含量测定 2 Fig. 2 Chromatogram of phytosterol standard 4, 2.6, 2.3, 4 2 2,, 4 β- 3, 4, 8512.06 mg/kg,,, 3~5 Table 1 表 1 4 种植物甾醇曲线方程 Curve equations of 4 kinds of phytosterols r (mg/l) Y=1.1233X-0.0212 0.9998 10 160 Y=1.0433X-0.0102 0.9997 10 160 Y=0.96393X+0.0019 0.9997 8 130 β- Y=1.01263X+0.0075 0.9999 20 400 Table 2 表 2 植物甾醇含量测定结果 (n=3) Phytosterol content determination results (n=3) (mg/kg) (mg/kg) (mg/kg) β- (mg/kg) (mg/kg) 2446.78 252.52 5812.76 8512.06 531.85 394.33 1200.91 2427.09 1377.52 215.79 2412.33 4005.64 : Fig. 3 3 Chromatogram of phytosterols in wheat germ oil
8, : 3391 Fig. 4 4 Chromatogram of phytosterols in soybean oil Fig. 5 5 Chromatogram of phytosterols in garlic oil 3.5 回收率及精密度试验,,, 3,, 3, 96.8% 101.3%, 3.0 %, GB/T 27404-2008( ) 3.6 稳定性试验, 0 4 8 12 24 48 h,, RSD 1.0%(n=6), 48 h 4 结论,,,,, 3 β-, β-,,,,,,,,
3392 7 Table 3 表 3 回收率测定 (n=3) Determination of the recovery (n=3) (mg) (mg) (mg) (%) (%) RSD(%) 0.6020 0.5949 101.19 β- 0.7525 0.7485 100.53 0.9030 0.8829 102.27 1.0028 1.0191 98.40 1.2535 1.2675 98.89 1.5042 1.5178 99.10 0.4460 0.4593 97.10 0.5575 0.5759 96.80 0.6690 0.6933 96.49 2.8360 2.8275 100.30 3.5450 3.5556 99.70 4.2540 4.1911 101.50 101.3 0.9 98.8 0.4 96.8 0.4 100.5 1.0 参考文献 [1] Moghadasian MH, Frohlich JJ. Effects of dietary phytosterols on cholesterol metabolism and atherosclerosis: clinical and experimental evidence [J]. Am J Med, 1999, 107(6): 588 594 [2] Kendrick M. The great choleaterol con [M]. London: John-Blake, 2008. [3] Nes WD. Biosynthersis of cholesterol and other sterols [J]. Chem Rev, 2011, 111: 6423 6451. [4] Daguer D. Phytosterol: highly promising compounds [J]. Lipid Tech, 2002, 12: 77 80. [5] Katan MB, Grundy SM, Jones P, et al. Efficacy and safety of plant stanols and sterols in the management of blood cholesterol levels [J]. Mayo Clinic Proceed, 2003, 78(8): 965 78. [6]. [J]., 2001, 28(5): 286. Han JH. The properties, functions and applications of phytosterol [J]. Foreign Med Hyg Pathol, 2001, 28 (5): 286. [7]..[M]. :, 2005. Tang CH. Sterol. Plant biological activity material [M]. Beijing: Chemical Industry Press, 2005. [8],. ( Ⅱ ) [J]., 2002, 27(03): 60 63. Wu SM, Wu MC. Advancement and tendency on phytosterol research ( Ⅱ ) Applied base and exploiture [J]. China Oils Fats, 2002, 27(03): 60 63. [9]. [J]., 1993, 2: 32 42. Chui YD. Physiological characteristics and its application of sterol [J]. J Cereals Oils, 1993, 2: 32 42. [10] Smith LL. Cholesterol autoxidation [M]. New York: Plenum Press, 1981. [11] Soupas L, Juntunen L, Lampi AM, et al. Effects of sterol stricture, temperature,and lipid medium on phytosteroloxidation [J]. J Agric Food Chem, 2004, 52: 6585 6491. [12] DeMan JM. Principles of Food Chemistry (2nd ed) [M]. New York: Van Nostrand Reinhold, 1990. [13] Bouic PJ. The role of phytosterols and phytosterolins in immune modulation: a review of the past 10 years [J]. Current Opinion Clin Nutr Metab Care, 2001, 4(6): 471 475. [14] Rudkowska I. Plant sterols and stanols for healthy ageing [J]. Maturitas, 2010, 66(2): 158 62. [15],,,. [J]., 2010, 31(15): 257 259. Song YQ, Wang SR, Wei ZW, et al. Wheat germ oil capsules antioxidant effect [J]. Food Sci, 2010, 27(15): 257 259. 作者简介 ( 责任编辑 : 白洪健 ) 张喜金, 主要研究方向为保健食品的质量检测 E-mail: 215865748@qq.coml