Microsoft Word 张涛-二校

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1 6 4 Vol. 6 No Journal of Food Safety and Quality Apr., 015 * 张涛, 胡旭, 程江南, 赵婷婷, 马媛, 张娟, 安熙强 (, ) 摘要 : 目的 方法 JJF ,, 结果 110 µg/ml, Y=73.966X+0.006, %, U=1.84%, (k=), 结论 关键词 : ; ; ; Determination of the content of polyunsaturated fatty acid in edible oil and evaluation of its uncertainty ZHANG Tao, HU Xu, CHENG Jiang-Nan, ZHAO Ting-Ting, MA Yuan, ZHANG Juan, AN Xi-Qiang * (The Xinjiang Institute of Meteria Medica, Urumqi , China) ABSTRACT: Objective To established an ultraviolet-spectrophotometry method for determination of the content of polyunsaturated fatty acid in edible oil, and a mathematical model of the uncertainty. Method Based on JJF Evaluation and expression of uncertainty in measurement, the main source of uncertainty were analyzed, and the uncertainty components were evaluated and calculated. Result The results showed that the linear range of polyunsaturated fatty acid in edible oil was 1~10 mg/ml, the linear equation was Y=73.966X (r=0.9998), and the expanded uncertainty was 1.84% (k=) when the content of polyunsaturated fatty acid was 56.1% in edible oil. According to analysis of measurement, the main sources of uncertainty were repetitive measurement, dispensing process of standard solution and the fitting of the standard curve. Conclusion This method can provide reference to evaluate quality of polyunsaturated fatty acid in edible oil. KEY WORDS: edible oil; polyunsaturated fatty acid; ultraviolet-spectrophotometry; uncertainty 基金项目 : ( ) Fund: Supported by the Xinjiang Uygur Autonomous Region High Technology Research and Development Project ( ) * 通讯作者 :,, @qq.com *Corresponding author: AN Xi-Qiang, Researcher, Xinjiang Institute of Meteria Medica, No 140, Xinhua South Road, Urumqi , China @qq.com

2 4, : 引言, (PUFA),, PUFA [1-4], PUFA,,,, [5] PUFA,,,,,, [6-8], [9-11] JJF [1], [13],, 材料与方法.1 材料与试剂 (); ( ); (, ); (, ); (, ); (, ); ( Sigma );. 仪器与设备 ML04 ( 0.1 mg, -); UV765 ( ).3 方法.3.1 样品处理 100 mg( 0.1 mg), 100 ml, 10 ml -,, 4 h, 0 ml 1.0 mol/l 10 ml,, 1 ml 100 ml, 0 ml 1.0 mol/l,, 0.1 ml, ml,.3. 多不饱和脂肪酸标准溶液的配制 160 mg, 100 ml, 0.1 mg ml 100 ml, 18 ml 1.0 mol/l,,, 0.1 mg/ml.3.3 补偿溶液的配制, 0.1 ml,.3.4 测定,, 35 nm 3 结果与分析 3.1 绘制标准曲线 ml, ml, 0. mol/l 0.1 ml 7, 3 ml ( ),, 35 nm Y Y X(mg/mL), Y=73.966X+0.006, r=0.9998, 1 3. 样品测定 ml, 35 nm,,

3 1454 6,, 1 1 Fig. 1 Polyunsaturated fatty acid concentration and absorbance standard curve 3.3 数学模型的建立 : cvf X 100 m : X (%); c (mg/ml); V (ml); f ; m (mg) 3.4 测量不确定度的主要来源, 1, 4- (GB/T ) [13], : (1) ; (); (3) ; (4); (5) 3.5 测量不确定度的评定 标准溶液配制引入的不确定度 : (1) 1.6%, k=, : u rel (P)= 1.6% = () mg,, k= : u 1 (m)= = mg 3, 0.5 [14] 0.1 mg, : u (m)= = mg,, : u(m)= u mu m 1 = mg m=160 mg, : u re1 (m)= um 1 m = = Table 1 表 1 食用油中多不饱和脂肪酸含量的测定结果 (n=6) Results of the content of edible oil polyunsaturated fatty acid (n=6) (mg) (mg/ml) (%) (%) RSD(%)

4 4, : 1455 (3) 1 JJG [15] 100 ml A ±0.10 ml( 3 ),, k= : 3, 100 ml u 1 (V 100)= = ml / [14], ±3, 100 ml : V 100= = ml 95%, k=1.96, : u (V 100)= V 100/k= /1.96= ml : u re1 (V 100)= u ( V容 ) u ( V容 ) /100= (4) 1 JJG [16] 10 ml A ±0.05 ml( 3 ),, k= : 3, 10 ml u 1 (V 10)= = ml / [14], ±3, 10 ml 10 ml : V 10= = ml 0.95, k=1.96, : u (V 10)= V 10/k= /1.96= ml 10 ml : u rel (V 10)= u ( V移 ) u ( V移 ) /10= ml,,, : u rel (f)= urel Pu re1 murel ( V容 100)+ urel ( V容 100) urel ( V移 10) = 样品称量引入的不确定度 (1) 0.1 mg,, k= : u 1 (M)= = mg 3, () 0.5 [14] 0.1 mg, : u (M)= = mg,, : u(m)= u Mu M 1 = mg M=100 mg, : u re1 (M)= u M 1 M = = 样品定容引入的不确定度 (1) 1 JJG [15] 100 ml A ±0.10 ml( 3 ),, k= : 3, 100 ml u 1 (V 100)= = ml / [14], ±3, 100 ml : V 100= = ml 95%, k=1.96, :

5 u (V 100)= V 100/k= /1.96= ml : u re1 (V 100)= u1 ( V ) u 100 ( V ) /100= 容容 100 () 1 1 ml A ±0.008 ml; ml A ±0.01 ml [16] ( 3 ),, k= 3, 1 ml : u 1 (V 1)=0.008/ 3 = ml u 1 (V )=0.01/ 3 = ml / [14], ±3, 1 ml : V 1= = ml V = = ml 95%, k=1.96, : u (V 1)= V 1/k= /1.96= ml u (V )= V /k= /1.96= ml : Table u rel (V 1)= u ( V移 ) u ( V移 ) /1= u rel (V )= u1 ( V移 ) u ( V移 ) /= ml,,, : u rel (V)= u ( V ) u ( V ) u ( V ) u ( V ) rel 容 100 rel 容 100 rel 移 1 rel 移 = 重复性测量引入的不确定度 1, (n=6): 6 ( xi x) i1 sx % 61 : s u(rep)= x n =0.6047% u rel (rep)= urep = % x 56.1% = 标准曲线拟合引入的不确定度, 表 曲线的残差计算结果 Calculation results of residual from the standard curve n c 0j (: mg/ml) A 0j ac 0j +b [A 0j -(ac 0j +b)] (c 0j - c 0 ) (: mg /ml ) c 0 =

6 4, : 1457 : n j A0 j ac0 b 4 j sr = = n 14 : 0 n ( c0 j c0) j1 sr 1 1 ( c c ) u line b p n ( ) = mg/ml : s r (); b ; p ; n ; c /(mg/ml); c0 j /(mg/ml); c0 /(mg/ml) : 5 uline urel line = c 合成标准不确定度 扩展不确定度及结果表述, : u rel = u f u M u V u rep u line rel rel rel rel rel = = : u=u rel X = %=0.904% k=, : U=k u= 0.904%=1.84% : (56.1±1.84)%, k= 4 讨论, 5558% [17-19],, GB/T , = [18-19],,,,, 参考文献 [1],,,. [J]. (), 014, 31(1): Yao SY, Liu T, Li R, et al. Research progress in polyunsaturated fatty acids and their anti-cancer role [J]. J Chongqing Technol Business Univ (Nat Sci), 014, 31(1): [],,,. [J]., 014, 1: , 158. Lang LW, Wang HY, Hu B, et al. Research advances of polyunsaturated fatty acids in cancer and inflammation disease [J]. Chin J Biochem Pharm, 014, 1: , 158. [3],,,. [J]., 013, 4(5): Zhang JY, Du B, Xie LH, et al. Progress of application of microencapsulation technology in polyunsaturated fatty acids [J]. J Food Saf Qual, 013, 4(5): [4],,,. [J]., 01, 33(7): Sun XY, Gao GT, Duan AL, et al. Research progress in polyunsaturated fatty acids [J]. Sci Technol Food Ind, 01, 33(7): [5],,. [J]., 1998, 13(3): 140. Chen ZN, Chen ZD, Wei ZH. Negative effect of vegetable Oil rich in PUFA and cultivar improvement of oil plant [J]. Fujian J Agric Sci, 1998, 13(3): 140. [6],,. [J]., 005, 1: 36. Li SG, Li XM, Chen H. Study on the status, the problem and the countermeasures of edible oil quality and safety in china [J]. Cereals Oils, 005, 1: 36. [7],,. [J]. (), 007, 8(4): Qi J, Yin GX, Luo H. Effect of vegetable oil polyunsaturated fatty acid (PUFA) on human s brain [J]. J Beihua Univ (Nat Sci),

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