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1 5 7 Vol. 5 No Journal of Food Safety and Quality Jul., 014 杨微微 1, 王俪瓯 1, 许乾丽, 胡立立 1, 杨园园 (1., ;., ) 摘要 : 目的 方法 -- (7::1), Waters Symmetry C 18 (50 mm 4.6 mm, 5 µm), 1.0 ml min -1, : 35, A, 0.0 mol L 1 1% 0.% (ph=4) B,,,,,, 结果,, 结论,,, 关键词 : ; ; ; ; Uncertainty analysis determination of citrine and sunset yellow in noodle by HPLC YANG Wei-Wei 1, WANG Li-Ou 1, XU Qian-Li, HU Li-Li 1, YANG Yuan-Yuan (1.Guiyang Medical University, Guiyang , China;. Guizhou Provincial Food and Drug Inspection Institute, Guiyang , China) ABSTRACT: Objective To establish a method for the determination and uncertainty analysis of citrine and sunset yellow in noodles by HPLC. Methods The samples was extracted by the solution of absolute ethyl alcohol, ammonia water and clear water (with the ratio of 7 1), and separated by liquid chromatographic column of Waters Symmetry C 18 column (50 mm 4.6 mm, 5 μm) flow rate 1.0mL/min, column temperature 35, using methanol-an aqueous solution of 0.0 mol/l ammonium acetate, 1% acetic acid and 0.% triethylamine(ph=4)as mobile phase. The factors of affecting the determination of citrine and sunset yellow were investigated, the sources of uncertainty were identified, the mathematic models were established, the components of uncertainty were calculated and the uncertainty was combined. Results The greatest influence on the combined uncertainty was the standard curve, the second influence on the combined uncertainty was the sample processing and the minimum influence on the combined uncertainty was the instruments. Conclusion 基金项目 : SY [011]3090 [01]4001 Fund: Supported by Guizhou Province Department of Project (Guizhou Branch SY Word [011] and 3090 Guizhou Branch Platform [01] 4001) and Country catering service project formulating food safety standards * 通讯作者 :,, @qq.com *Corresponding author: XU Qian-Li, Professor of Pharmacy, Guizhou Provincial Food and Drug Inspection Institute, No.14, Shibei Road, Guiyang , China @qq.com

2 7, : 09 The HPLC method is objective and accurate for determination and uncertainty analysis of citrine and sunset yellow in noodles and calculation of uncertainty in the experimental method of content. It has strong practicability in the practical work. KEY WORDS: noodle; citrine; sunset yellow; content; uncertainty 1 引言,,,,,,, [1-3],,, [4],,,,, [5-6] [5-1], [13-16],, 材料与方法.1 材料与仪器 ( 90.0%, Dr. Ehrenstorfer GmbH ); ( 87.0%, Dr. Ehrenstorfer GmbH ); (, ); (, ); LC-010AHT (); ; XS05 BT0S ( Sanorius ); KQ500DE ( ); 0.45 μm ( ). 实验方法..1 对照品溶液的制备 g g 100 ml,,, μg/ml μg/ml ml 5 ml.. 供试样品溶液的制备 ( )4.00 g, 100 ml, -- (7::1) 80 ml, HZ 30 min,,, -- (7::1),,, 10 ml, 0 ml,, 5 ml,,, (5000 r min 1, 5 min),..3 色谱条件 : Waters Symmetr C 18 ( 50 mm 4.6 mm, 5 µm); 45 nm 483 nm : 35 ; A, 0.0 mol L 1 1% 0.% (ph=4) B, ; 1.0 ml min 1 ; DAD ; : 10 μl 3 结果与讨论 3.1 建立数学模型 A=ac+b (1) c v ω = () m L a b,, r(a, b) 1, [17] (3) (4),

3 10 5 C C C C C u C u A u u b r a b A a b a b ( ) = ( ) + ( a) + ( ) + (, ) 1 A b 1 A b 1 = u( A) u( a) u( b) u( a) u( b) a u a a a 1 A b 1 = u( A) u( a) u( b) a + u a (3) ω ω ω ω u( ω) = u( C) + u( v) + u( m) + u( L) C v m L V C v C v C = u( C) u( v) u( m) u( L) m L m L m L m L : A, a, b, c, µg/ml, ω (mg/kg), V, L 0 ml/100 ml, m (g) 3. 不确定度分量计算 3..1 称量过程引入的不确定度 u(m),, 0.01 g, (), u(m)= g=.900 mg 3.. 定容过程引入的不确定度 u(v) :, u 1, x x(ml),, u 1= ml; 3, (1 ) (4 ), 3 ( 1, 4, 3 ), ml/ 4, u = v ml;, 3 1 % u 3 = : u v = u1 + u + u3 (5) : u 5 = ml u 100 = ml 3..3 标准系列溶液浓度定值的不确定度 u A-1 (4), u (m 1 ); u (m ); u (f); u (v) (1) u (m 1 ), ±1 % ± % k=, u (m 1 )= 0.01 a( )=15.76A; u (m 1 )= 0.01 a( )=99.18A (a, 1 ) () u(m ) g, g,,, 0.01mg, (), u( )= /13.51=0.01 ; u( )= /43.3= u (m )=0.01 a( )=6.56A; u (m )= a( )=.00A (3) u (f) 5 ml, ±0.015 ml; (5) 5 ml : u= u1 + u + u3 =0.0098, u r = =0., 5

4 3 7, : 11 u (f)=0. a( )=61.10A; u (f)= 0. a( )=59.84A (4) u (v) 1 5 ml u (v 1 ) 5 mla, ±0.03 ml, (5) 5 ml : u r = u1 + u + u3 =0.00, u= 0.00 =0.08, 5 u (f)=0.08 a( )=4.44A; u (f)= 0.08 a( )=3.93A 100 ml u (v ) (5) 100 ml ml, u= = 0.068, u (f)=0.068 a ( )=0.78A; u (f)= 0.068% a ( )=0.34A u A-1 = : 标 ( ) + u标 ( m ) + u( f ) + u标 ( v ) u ( v ) u + m1 1 标 u A-1( ) =167.75A; u A-1( )=306.7A 3..4 高效液相色谱仪测得峰面积的不确定度 u A- ;, LC-0A 0.4%,, u A- = 0.4% 3 =0.003A 3..5 残差的标准不确定度 u A-3, 1, 10 μl u A-3 u A 3 k k ( Aji Ai ) i= 1 j= 1 = S = k n k, n u A-3( ) = / u A-3( )= 表 1 柠檬黄标准品测量结果 Table 1 The results of reference substance for citrine μg/ml A ij A Â a= b= r= 表 日落黄标准品测量结果 Table The results of reference substance for sunset yellow μg/ml A ij A Â a= b= r=

5 1 5 u ( ) A=[ u A-1( ) + u A-( ) + u A-3( )] 1/ = 636.9A u ( ) A=[ u A-1( ) + u A-( ) + u A-3( )] 1/ = A 3..6 斜率的标准不确定度 u a 1/ 1 u( a) = s n ( ci ci) i= 1 u a( )=65.30 u a( )= 截距的标准不确定度 u (b) u a( )=73.63 u b( )= 分取比 L 的不确定度 u(l) ml 0.068; 0 ml, ±0.03 ml, u 0 =0.019 ml : L=V 0 /V 100 u L V ( L ) = u ( V ) + u ( V ) u(l)= L V 被测溶液中柠檬黄 日落黄浓度测量准不确定度 (3) u(c) =0.01 µg/ml u(c) =0.074 µg/ml 3.4 被测样品溶液中柠檬黄 日落黄含量不确定度为 u(ω), 3, µg/ml, 1.34 µg/ml, (4), u (ω)=0.078 mg/kg, u (ω)=0.47 mg/kg 3.5 结果 95% k=, u =0.078 =0.16mg/kg, u 日落黄 =0.47 =0.94mg/kg;, 3, 4.61 mg/kg, 8.33 mg/kg ω =.61 ± 0.16(mg/kg); ω 日落黄 =8.33 ± 0.94 (mg/kg) k= (g) A 表 3 柠檬黄 6 次测量的结果 Table 3 Citrine 6 times measurement results C C C(µg/mL) C X (mg/kg) 表 4 日落黄 6 次测量的结果 Table 4 Sunset yellow 6 times measurement results (g) A C C C C X (mg/kg)

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7 14 5 Zhang JB, Zhu LH, Lin L. Determination of phosphorus,iron,zirconium and niobium in titanium pigment by X-ray fluorescence spectrometry [J]. Metall Anal, 009, 9(1): [16],. [M]. :, 006. Conformity assessment in China national center for recognition and institute of Baoshan iron and steel company compile. Material physical and chemical inspection measurement uncertainty evaluation guidelines and examples [M]. Beijing: China Metrology Press, 006. [17]. [M]. :, 000. Thestate bureau of quality and technical supervision measurement department.measurement uncertainty evaluation and guide said [M]. Beijing: China Metrology Press, 000. 作者简介 ( 责任编辑 : 杨翠娜 ) 杨微微, 在读研究生, 主要研究方向为食品药品质量研究 @qq.com 许乾丽, 主任药师, 主要研究方向为食品药品质量研究 @qq.com 功能性食品研究 专题征稿 tougao@chinafoodj.com 食品安全质量检测学报 编辑部