Microsoft Word 高宏-二校-有修改

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1 6 1 Vol. 6 No Jornal of Food Safety and Qality Jan., 2015 高宏 *, 徐慧, 郭芳芳, 李青 (, ) 摘要 : 目的 GB/T , (gas chromatography, GC) 方法 GC,,,,, 结果 , (5.21±0.79) μg/kg, (4.9±0.56) μg/kg; 结论关键词 : ; ; ; Evalation of ncertainty of aldrin and dieldrin in milk GAO Hong *, XU Hi, GUO Fang-Fang, LI Qing (Jiangs Test Center for Physics and Chemistry, Nanjing , China) ABSTRACT: Objective To evalate the test reslts of ncertainty of aldrin and dieldrin detected by gas chromatography(gc) in milk, according to GB/T Determination of organo chlorine pesticides in foods mlticomponent resides. Methods The factors affecting the ncertainty were dedced by establishing mathematical model for the determination by GC method. Each component of ncertainty was evalated and calclated, from which the combined ncertainty and the extended ncertainty were obtained. Reslts The combined ncertainty of aldrin and dieldrin in milk for determination was and 0.059, and the determined content of aldrin and dieldrin was (5.21±0.79) μg/kg and (4.9±0.56) μg/kg, respectively. The standard crve, pre-treatment process and instrment measrement repeatability was the primary factor for determination of aldrin and dieldrin. Conclsion The establishment of the methodology for the evalation of measrement ncertainty is important for the determination of aldrin and dieldrin pesticides in milk. KEY WORDS: milk; aldrin; dieldrin; ncertainty 1 引言 (aldrin)(dieldrin) [1], * 通讯作者 :,,, @qq.com *Corresponding athor: GAO Hong, Intermediate Engineer, Jiangs Test Center for Physics and Chemistry, Nanjing , China @qq.com

2 16 6, [2] 2001 (POPs), [],, [4], [5-7], [8] (JJF ) [9],,,,, 2 材料与方法 2.1 仪器与试剂 Agilent 7890B, (ECD) OpenLAB CDS ( ); HZQ-100A ( ); EYELA SB-2000 ( ); MTN-2800W ( ) (, ) (), 100 μg/ml 2.2 色谱条件 : BR-5, 0 m 0.25 mm, i.d. 1.0 μm df : 80 2 min 10 /min 250 min, 10 /min min; : 00 ; : 270 : 99.99%, ; : 1 ml/min; : 0 ml/min; : 1 μl; : 2. 标准系列溶液的配制 1.0 ml, 10 ml,, 10 μg/ml 1 ml 10 ml,, 1 μg/ml, ng/ml 2.4 样品的处理 ()500 g 20 g ( 0.01 g), 0 ml, 0 min 6 g,, 0 ml, 0 min,, 5 ml 10 ml, + (1:1, v:v),,, 5 ml 2.5 样品的测定 1 μl,,, 数学模型, : cv f X Frep m R ec : X:, mg/kg; c:, μg/ml; V:, ml; f: ; m:, g; R ec : ; F: ; rep: 4 不确定度来源分析,, : (1) () ; (2) ;

3 1, : 17 () ; (4) ; (5) ; (6) ; (7) 5 不确定度分量的评定 5.1 标准溶液及配制过程 ( 稀释定容 ) 中引入的不确定度 (m 1 ) 标准溶液的不确定度 B,, 100 μg/ml, 0.10 μg/ml 0.08 μg/ml P=95%, k=2, (c 艾氏剂 ) , (c 狄氏剂 ) 标准溶液配制过程引入的不确定度 (1) 125 ml, JJG , 125 ml A ±0.007 ml±0.010 ml±0.015 ml,, k=,, ( V 吸 2) ; ( V 吸 1) ; ( V 吸 ) (2) 20±2,, ml/,, ( V 吸 1) ; ( V 吸 2 ) ; ( V 吸 ) () 1 ( 吸 1 2 ( 吸 1 V ) V ) ( V吸 1) 0.004; 1 1 ( 吸 2 2 ( 吸 2 V ) V ) ( V吸 2 ) 0.002; 2 1 ( 吸 2 ( 吸 V ) V ) ( V吸 ) (1) 10 ml, JJG , 10 ml A ±0.020 ml,, k=, 0.020, 1 ( V 容 1) = = (2) ±2,, ml/,, ( V 容 1) = = () 1 ( 容 1) 2 V ( V容 1) = = 标准溶液及配制过程 ( 稀释定容 ) 中引入的相对不确定度, 125 ml 214, 10 ml 7, : 艾氏剂 ( c ) ( V吸 1) 2 ( m1 ) ( V ) ( V ) 4 ( V ) 7 2 吸 2 吸容 1 (m 1 ) 标准曲线引入的不确定度 (m 2 ) ng/ml,,,, :

4 18 6 SR 1 1 ( cx c) c ( x ) ; b p n 2 ( c c) n i i i1 i1 y ( bc a) 2 SR n 2, S R ; ab ; p, p=2; n, n=5; c x ; c i ; c, c =77.5 μg/l, y i i 2.5, GB mg/kg, 24 ng/ml, c x () ng/ml, c x () ng/ml S R, S R ()= ng/ml, S R ()= ng/ml 2 c x c S R (c x ), (m 2 ) i 2 5. 样品的非均匀性引入的不确定度 (m ) F rep, F 1,,,,, (m ) 样品称量引入的不确定度 (m 4 ) g, A, ±0.1 mg,, k=, m ( 4 ) , (m 4 )= 样品处理后定容引入的不确定度 (m 5 ) 5 ml, 5 ml A ±0.015 ml,, k, m ( 4) , (m 5 )= 样品前处理过程引入的不确定度 (m 6 ),,, 6, H, Table 1 表 1 艾氏剂狄氏剂标准系列溶液测定结果 Measrement reslts of standard series soltion of aldrin and dieldrin (ng/ml) Y=54.5C Y=291.1C Table 2 表 2 艾氏剂狄氏剂标准曲线引入的相对不确定度 (m 2 ) Relative ncertainty introdced by standard crve of aldrin and dieldrin c x (ng/ml) c (ng/ml) S R (ng/ml) c ( x) (ng/ml) ( m 2)

5 1, : 19 Table 表样品前处理过程引入的相对不确定度 (m 6 ) Relative ncertainty introdced by the sample preparation process. (μg/kg) H 1 (%) H 2 (%) H (%) s(h)(%) (m 6 ) 表 4 6 份模拟样品中农药残留测定结果 Table 4 Reslts of pesticide resides in 6 samples c s(c) (m 7 ) (μg/kg) (μg/kg) 测量重复性引入的不确定度 (m 7 ), GB mg/kg, 6 6 (n=6), 4, 5.8 相对合成标准不确定度和相对扩展不确定度,, : c c ( 1 ( 2 ( ( 4 m) m) m) m) ( w艾氏剂 ) m) m) m) 2 ( 5 ( 6 ( 7 ( 1 ( 2 ( ( 4 m) m ) m) m ) ( w艾氏剂 ) m) m ) m ) 2 ( 5 ( 6 ( 7 k=2, 95%, : U( w ) 2 ( w ; 艾氏剂 c 艾氏剂 ) U( w狄氏剂 ) 2 c ( w狄氏剂 ) 讨论 (1),,,, (2),,, [10,11] [12], [1,14], [15] (),,, 参考文献 [1],,,. - [J]. (), 2011, 4(4): Pang YH, H XJ, Sn XQ, et al. Determination of reside in food of aldrin and dieldrin gas chromatography-mass spectrometry [J]. J Liaoning Normal Univ (Nat Sci Edit), 2011, 4(4): [2]. [J].,

6 , 10: 212. Sn HX. Research on persistent organic polltants [J]. Exp Teachnol App, 2014, 10: 212. []. [J]., 2014, 4(10): H QH. Occrrence and ecological risk assessment of persistent organic polltants in Meizho bay [J]. Chin Environ Sci, 2014, 4(10): [4],,,. [J]., 2010, 22(): Zho PP, Zh LP, Zhao YF, et al. Analysis on persistent organochlorine pesticide mltiresides in animal origin foods [J]. Chin J Food Hyg, 2010, 22(): 19198, [5],,. [J]., 201, 22(5): Li J, Wang L, Zeng XY. Evalation of measrement ncertainty of endrin in seawater by GC with solid-phase extraction [J]. Chem Anal Metrol, 201, 22(5): [6],.,. - [J]., 2014, 5(12): Wang JX, Zhang XZ, Wang YQ, et al. Uncertainty evalation for the determination of bifenthrin in tea by gas chromatography and gas chromatography-mass spectrometry [J]. Food Sci, 2014, 5(12): [7],,,. [J]., 2012, 2(2): Ying F, Lan DD, X JF, et al. Evalation of ncertainty of measrement oforganochlorine pesticides in water [J]. Agric Technol, 2012, 2(2): [8],,,. [J]., 2005, 11(2): Liang KL, Jiao TS, Li SB, et al. Measrement ncertaing in analytical data processing [J]. Anal Test Technol Instrm, 2005, 11(2): [9] JJF [S]. JJF Evalation and expression of ncertainty in measrement [S]. [10],,,. -- [J]., 2009, 28(1): 8. H BZ, Shen GJ, Shao TF, et al. Determination of organochlorine and pyrethroid pesticide resides in tea by accelerated solvent extraction and gas chromatography negative chemical ionization-mass spectrometry [J]. Chin J Anal Lab, 2009, 28(1): 8. [11] JJF [S]. JJF Evalation of ncertainty in chemical analysis measrement [S]. [12]. [S]. Beijing environmental protection monitoring center. Evalation of ncertainty in measrement of environmental monitoring [S]. [1]. GC 5 [J]., 2014, 1: Chen JQ. Evalation of measrement ncertainty for determination of five organochlorine pesticide resides in glycyrrhizae radix Et rhizoma by GC [J]. Chin J Mod App Pharm, 2014, 1: [14],,. [J]., 2014, 1(1): Y XZ, Xiong DQ, Zhang LL. Vale of ncertainty evalation index and qality goal index in evalating the qality of conventional chemical test reslts [J]. Mod Prev Med, 2014, 1(1): [15],,,. [J]., 2010, 12(): Li RS, Wang Y, W NY, et al, Uncertainty evalation in assay of ethanol in shi-di-shi tinctre by capillary GC method [J]. Prog Pharm Sci, 2010, 12(): 作者简介 ( 责任编辑 : 杨翠娜 ) 高宏, 硕士研究生, 中级工程师, 主要研究方向为食品安全分析测试 @qq.com

Microsoft Word 邹游二校

Microsoft Word 邹游二校 7 6 ol. 7 No. 6 016 6 Jornal of Food Safety and Qality Jn., 016 - 邹游 *, 蓝草, 欧阳少伦, 邵琳智, 林峰 (, 5106) 摘要 : 目的 - 方法 GB/T 88-008, CNAS-GL06: 006,, 结果 50 μg/kg,.70 μg/kg(k=), 结论, 关键词 : -; ; ; ; Uncertainty evalation