Microsoft Word 李 莹-二校.doc

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1 6 11 Vol. 6 No Journal of Food Safety and Quality Nov., 李莹 *, 付骋宇, 何强, 孔祥虹, 李建华 (, ) 摘要 : 目的 方法 -,,, 结果 μg/ml, , 78.6%, 79.2%, 78.3%, 79.6% 1.0 mg/kg 结论, 关键词 : ; ; ; ; ; Simultaneous determination of 4 colorants in meat products by high performance liquid chromatography LI Ying *, FU Cheng-Yu, HE Qiang, KONG Xiang-Hong, LI Jian-Hua (Shaanxi Entry-Exit Inspection and Quarantine Bureau, Xi an , China) ABSTRACT: Objective To establish a method for the determination of 4 colorants (allure red AC, carmosine, tartrazine, sunset yellow FCF) in meat products by high performance liquid chromatography (HPLC). Methods The sample was extracted by the solution which was made up by ammonium hydroxide and ethanol and degreased by n-hexane, then concentrated by sample concentrator. The sample was detected by HPLC with UV detector. Results This method showed a good linearity in the range of 0~50.0 μg/ml(r ). The average recovery were 78.6%, 79.2%, 78.3%, and 79.6% for allure red AC, carmosine, tartrazine, and sunset yellow FCF, respectively. The detection limit was 1.0 mg/kg for all. Conclusion The method is simple, rapid and high sensitive, which can be used for the detection of allure red AC, carmosine, tartrazine, sunset yellow FCF in meat products. KEY WORDS: allure red AC; carmosine; tartrazine; sunset yellow FCF; meat product; high performance liquid chromatography 1 引言 [1-3],, [4-7], 基金项目 : ( K ) Fund: Supported by Shaanxi Entry-Exit Inspection and Quarantine Bureau Project (K ) * 通讯作者 :,,, crystal.zero@163.com *Corresponding author: LI Ying, Engineer, Shaanxi Entry-Exit Inspection and Quarantine Bureau. No.10 Hangang North Road, Beilin District, Xi an , China. crystal.zero@163.com

2 11, : , GB ,, [8-16], GB/T , SN/T , GB/T ,,,,, 2 材料与方法 2.1 仪器与设备 Agilent 1260 ( Agilent ); XP204 (Mettler ToleDo ); HCB602H ( (), 0.01 g); HS 501 digital IKA-WERK E ( IKA ); BuChi Syncore (); Centrifuge 5810R (Eppendorf ) 2.2 材料与试剂 (, ); (HLPC, TEDIA ); (, ); (, ); (, ) -(V:V=7:3): 700 ml, 300 ml 0.02% : 1.54 g 1000 ml, ph 6.5, : 0.02 mol/l ( PH 6.5)-(V:V=3:7) 2.3 实验方法 标准溶液的配制 : 0.5 mg/ml : 0.5 mg/ml 4, 100 μg/ml, -4, 样品制备方法 5.0 g, - (V:V=7:3)20 ml, 10 ml 15 min, 4500 r/min 5 min,,, 40, 80 psi, -5 3 ml, 15 ml,, 8 ml, 4500 r/min 5 min, HPLC 测定条件 : Inertsil ODS-sp (4.6 mm 250 mm, 5 μm); : -0.02% (ph=6.5), 1, : 表 1 梯度洗脱程序 Table 1 Program of gradient elution (min) (ml/min) (%) 0.02% (ph=6.5)(%) : vis, nm, 4 nm min 440 nm, 6.5~22 min, 505 nm : 40, : 20 μl,, HPLC 1

3 Fig Chromatogram of 4 mixed standards solution 2.4 数据处理,, 3 结果与讨论 3.1 样品前处理条件的选择 GB/T (:: =7:2:1)(V:V:V), :=7:3(V:V),, :=7:3(V:V) 3.2 色谱柱和流动相的选择, ODS-3 ODS-SP, ODS-3, ODS-SP ODS-SP GB/T % ph, 3.3 检测器参数的选择 DAD 254 nm,, nm 481 nm 508 nm 510 nm, 4,, 0~6.5 min, 440 nm, 6.5 min 505 nm,, 3.4 线性范围 相关系数与检出限 μg/ml 4 Y, X(μg/mL), (S/N=10), mg/kg 3.5 回收率与精密度 μg/kg,, 6,, 3

4 11, : Table 2 表 2 4 种色素回归方程 线性范围及检出限 Regression equation, linear range and detection limit of the 4 colouring agents r μg/ml mg/kg Y=59.62X Y=49.61X Y=58.13X Y=54.77X Table 3 表 3 样品回收率实验 (n=6) Recovery experiments of samples (n=6) (μg/kg) (%) (%) RSD(%) ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ 方法的应用, 133, 1, 1.8 μg/kg, 1, 1.4 μg/kg, 1, 1.5 μg/kg, 11, 13~3.4 μg/kg, DAD,,

5 结论,,, 4,,,,, 参考文献 [1],,,. HPLC [J]., 2014, 43(6): Zeng YM, Chen FH, Liu ZH, et al Determination of non-fermented bean products by double wave-length HPLC [J]. Appl Chem Ind, 2014, 43(6): [2],,, / - 12 [J]., 2014, 33(5): Qian XY, Liu HS, Zhu XY, et al. Simultaneous determination of 12 synthetic colorants in cosmetics by SPE/UPLC-MS/MS [J]. J Instrum Anal, 2014, 33(5): [3], 6 [J]., 2014, 8:47 50 Hu LZ, Zhang YF. Simultaneous determination of six colorants in cigarette wrapping materials by high performance liquid chromatography [J]. Tob Sci Technol, 2014, 8: [4]. 3 [J]., 2014, 2: Zhang ZR. Determination of 3 colorants in plum meat by HPLC [J]. Mod Sci Instrum, 2014, 2: [5],,,. - 4 [J]., 2014, 6: Xiao L, Yu ZF, Xue F, et al. Simultaneous determinationof four synthetic colorants in dried shrimps by polyamide cartridge and HPLC [J]. China Food Addit, 2014, 6: [6],,,. 38 [J]., 2015, 33(3): Mao XQ, LI CL, Ren GJ, et al Simultaneous determination of 38 limited colorants in cosmetics by high performance liquid chromatography [J]. Chin J Chromatogr, 2015, 33(3): [7],,,. 8 [J]., 2015, 42(7): Zhang DF, Zhu AL, Tao HX, et al Simultaneous determination of 8 kinds of synthetic colorants in maize flour and wheat flour by HPLC [J]. Mod Prev Med, 2015, 42(7): [8],,,. / - 29 [J]., 2011, 29(7): Zhao YS, Yang ML, Zhang F, et al. Screening method for 29 forbidden or limited synthetic pigmentsin cheese by liquid chromatography/quadrupole time-of-flight mass spectrometry[j]. Chin J Chromatogr, 2011, 29(7): [9],,,. 46 [J]., 2012, 40(2): Zhao YS, Dong Y, Zhang F, et al. A study on system of sequential extraction and cleaning of 46 forbidden and limited synthetic pigments in food stuff [J]. Chin J Anal Chem, 2012, 40(2): [10],,,. [J]., 2008, 8(1): Lin CX, Fu B, Li HH, et al. Detection of fancy red stearic sugar from candy with high performance fiquid chromatography [J]. J Trop Med, 2008, 8(1): [11],,,. [J]., 2005, 5(3): Lin CX, Zeng HH, Fu B, et al. Detection of artificial pigment from meat products by using high performance liquid chromatography [J]. J Trop Med, 2005, 5(3): [12]. -HPLC [J]., 2015, 2: Chang H. Determination of synthetic pigments in foods by automatic solid-phase extraction-hplc [J]. Anhui J Prev Med, 2015, 2: [13],,,. [J]., 2009, 30(5): Liu CL, Li XQ, Wang J, et al Research Pprogress on rapid detection of azo-compound inedible pigment [J]. Food Sci, 2009, 30(5): , [14],,,. 7 [J]., 2014, 21(6): Zhou R, Mou RX, Xu P, et al. Determination of 7 synthetic pigments in food by HPLC [J]. Cereal Food Ind, 2014, 21(6):

6 11, : ( 责任编辑 : 白洪健 ) [15] GB/T [S] GB/T Determination of synthetic colour in foods [S]. 作者简介 [16],,,. 9 [J]., 2014, 23: Wang ZY, Tan Y, Wang TJ, et al. Determination of nine artificial 李莹, 硕士, 工程师, 主要研究方向为食品安全色谱检测的研究 crystal.zero@163.com pigments in meat products by high performance liquid chromatography [J]. Chin J Health Lab Technol, 2014, 23: