Microsoft Word 路杨-二校 647

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1 6 2 Vol. 6 No Journal of Food Safety and Quality Feb., 2015 路杨 1, 杨立新 1,2, 刘印平 1, 王丽英 1, 董彬 1, 常凤启 1 (1., ; 2., ) 摘要 : 目的 10 方法,, 10, 结果,, 56.0%~96.4% 70.0%~98.2%, (n=6) 1.9%~8.2% 1.8%~7.9%, (S/N=3) 0.009~0.051 mg/kg, (S/N=10) 0.030~0.153 mg/kg 结论,, 关键词 : ; ; ; ; Determination of 10 dyes in hotpot material and chill by ultra performance liquid chromatography with gel permeation chromatography cleanup LU Yang 1, YANG Li-Xin 1,2, LIU Yin-Ping 1, WANG Li-Ying 1, DONG Bin 1, CHANG Feng-Qi 1 (1. Hebei Center for Disease Control and Prevention, Shijiazhuang , China; 2. College of Environmental Science and Engineering, Peking University, Beijing , China) ABSTRACT: Objective To establish a method for the determination of 10 dyes in hot pot material and chili oil. Methods Ten dyes in chili oil, hotpot material and other foods with abundant fat were detected by gel permeation chromatography (GPC) with ultra performance liquid chromatography (UPLC). At the same time the effectiveness was verified. Results Spiking experiments were carried out in high, medium and low level, respectively. Recoveries of chili oil and hotpot material were between 56.0%~96.4% and 70.0% to 98%, the (n=6) were between 1.9% to 8.2% and 1.8% to 7.9%, the limits of detection (S/N=3) were between 0.009~0.051 mg/kg, and the limits of quantification (S/N=10) were between 0.030~0.153 mg/kg. Conclusion This method is simple to operate with good stability and is suitable for the application in daily testing work. KEY WORDS: dye; gel permeation chromatography; ultra performance liquid chromatography; chili oil; hotpot material 基金项目 : (JB D)( ) Fund: Supported by the Platform Construction Project of Hebei Science and Technology Department (JB D) and the Technology Support Project of Langfang City ( ) * 通讯作者 :,, yanglixin241@163.com *Corresponding author: CHANG Feng-Qi, Chief Technician, Hebei Center for Disease Control and Prevention, No.97, Huaiandonglu Road, Yuhua District, Shijiazhuang , China. yanglixin241@163.com.

2 引言,, [1], Ⅰ~Ⅳ [2-4],,, [5,6] [7-9], [10], [11-13], [14,15],, (solid phase extraction, SPE) [16-17] (matrix solid-phase dispersion, MSPD) [18-20],,,,,, [21] (gel permeation chromatography, GPC),, GPC (ultra performance liquid chromatography, UPLC) 10 2 材料与方法 2.1 仪器与试剂 DAD (Acquty UPLC, Waters ); (AccuPrep MPSTM, JZ Scientific ); 25 g Bio-Beads S-X3 300mm20 mm (MMS-310, EYELA ); (N-1001, EYELA ); (G560E, Scientific Industries ); (Ⅲ, Associaes ); (KQ-600E, );, 0.22μm,,, (, Thermo fisher, ); Mili- Q : Ⅰ~Ⅳ, 7B, B, B, G,,, Dr. Ehrenstorfer GmbH, 99.5% 2.2 溶液的配制 : 10 ml,,, 1000 μg/ml, 18 : 100 μl 10 ml,, 10 μg/ml, 4 :, :(90:10, v:v) ,, CAS, 仪器条件 : Waters BEH C 18 (2.1 mm 100 mm, 1.7 μm), A, B (0.01 mol/l) 0.1%: 0 min, A 30%, 3.0 min, 60%, 3.3 min 95%, 95% 8.9 min, 9.0 min, 30% 4 µl 0.3 ml/min, 样品前处理样品提取 0.5 g 15 ml, :(1:1, v:v) 10 ml, 1 min, 30 min, 0.22 μm, 样品净化 GPC, 5 ml, 254 nm, -(1:1, v:v), 5 ml/min, 13.5 min, 13.5~20 min, GPC 5 min, 1 ml,, UPLC

3 2, : Table 1 表 1 目标化合物中英文名称 CAS 编号分子量及使用液浓度 The Chinese name, English name, CAS NO., MW and concentration of target compounds CAS (μg/ml) Sudan Orange Para red G Sudab red G I Sudan I II Sudan II III SudanIII IV Sudan IV B Sudan red 7B B Rhodamine B B Sudan red B 样品分析 UPLC, 2,,, 3 结果与讨论 3.1 GPC 条件的优化 GPC 10 mg/l 10 GPC, 5.0 ml/min, 25 min, 13.5 min, 20 min ; 5~12 min, 13.5~20 min GPC 25 min,, GPC, GPC 加标回收率检出限和定量限 3 ( 3),, () %~96.4% 61.0%~98.2%, (n=6) 1 GPC Fig. 1 GPC chromatogram of oil 1.9%~8.2% 1.8%~7.9% (S/N) 3 (S/N) 10, 0.009~0.051 mg/kg, 0.030~0.153 mg/kg ( 2) 样品测定 30 1, 3.3%,,

4 , UPLC B mg/kg, (liquid chromatography tandem mass spectrometry, LC- MS/MS), LC-MS/MS B mg/kg, Table 2 表 2 目标化合物保留时间检测波长线性范围相关系数检出限和定量限 The retention time, detection wavelength, the linear range, correlation coefficient, detection limit (LOD) and quantitation limit (LOQ) of target compounds (min) (nm) (µg/g) (µg/g) (µg/g) ~ ~ G ~ I ~ II ~ III ~ IV ~ B ~ B ~ B ~ Fig. 2 The chromatogram of standard solution diluted 20 times a: 430nm ; b: 490nm ; c: 520nm 1. ; 2.; 3. G; 4. I; 5. II; 6. B; 7. III; 8. 7B; 9. B; 10. IV a: the detection wavelength was 430 nm; b: the detection wavelength was 490 nm; C: the detection wavelength was 520 nm 1. Sudan yellow; 2. para red; 3. Sudan red G; 4. Sudan red I, 5.Sudan red II; 6. Rhodamine B; 7. Sudan red III; 8. Sudan red 7B; 9. Sudan red B; 10. Sudan red IV

5 2, : Table 3 表 3 辣椒油及火锅底料低中高水平加标回收实验结果 The recovery tests results of chili oil and pot bottom material in low, medium and high levels (μg/ml) G I II B IV 7B B III Fig. 3 Chromatogram of positive sample 4 结论, ( PDA ),,,,, 参考文献 [1]. [J]., 2005, 32(3): Song Y. Risk assessment of Sudan red in food [J]. Foreign Med Sci (Sec Hyg), 2005, 32(3): [2],,. [J]., 2011,36(3): Zhang JY, Wu JE, Chang C. Research progress of toxicology of malachite green [J]. Grain Sci Technol Econ, 2011,36(3): [3] Johnaon GE, Quick EL, Parry EM, et al. Metabolic influences for mutation induction curves after exposure to Sudan-1 and Para red [J]. Mutagenesis, 2010, 25(4): [4] Rao KV. Toxicity and metabolism of malachite green and leucomalachite green during short term feeding to Fischer 344 rats and B6C3F1 mice [J].Chemico-Biol Inter, 2007, (122): [5],,,. [J]., 2012, 28(09): Zheng YM, Guo W, Nie XM, et al. Research on detection

6 652 6 methods of inedible pigment illegally added to food [J]. Chin Agric Sci Bull, 2012, 28(09): [6] Kucharska M, Grabka J. A review of chromatographic methods for determination of synthetic food dyes [J]. Talanta, 2010,80: [7],,,. 1 [J]., 2007, 38(8): Han D, Yu M, Wu M, et al. A Sensitive enzyme linked immunosorbent assay for the analysis of sudan in food samples [J]. Chin J Anal Chem, 2007, 38(8): [8],,,. Ⅰ ELISA [J]., 2010, 24(2): Zhang MZ, Fang JH, Cheng ZL, et al. Development of direct competitive elisa kit for sudan [J]. J Nuclear Agric Sci, 2010, 24(2): [9] Chang XC, Hu XZ, Li YQ, et al. Multi-determination of Para red and Sudan dyes in egg by a broad specific antibody based enzyme linked immunosorbent assay [J]. Food Control, 2011, (22): [10],,,. - ⅠⅡ[J]. -, 2006, 42(12): Su XC, Huang M, Gan BB, et al. GC-MS determination of the pigments Sudanand Sudan in some flavourings [J]. Phy Test Chem Anal Part B: Chem Anal, 2006, 42(12): [11] Javorsek D, Kovac F, Gorensek M. HPLC analysis of monofluoro-s-triazine dye during the dyeing process [J]. Am J Anal Chem, 2014, 5: [12] Ertas E, Ozer H, Alasalvar C. A rapid HPLC method for determination of sudan dyes and para red in red chilli pepper [J]. Food Chem, 2007, 2(105): [13] Khanavi M, Hajimahmoodi M, Ranjbar AM. Development of a green chromatographic method for simultaneous determination of food colorants[j]. Food Anal Method, 2012, 5: [14] Cornet V, Govaert Y, Moens G, et al. Development of a fast analytical method for the determination of sudan dyes in chilliand curry-containing foodstuffs by high-performance liquid chromatography photo-diode array detection [J]. J Agric Food Chem, 2006, 54: [15] Ma M, Luo X, Chen B, et al. Simultaneous determination of water-soluble and fat-soluble synthetic colorants in foodstuff by high-performanceliquidchromatography-diodearraydetection-elec trospray mass spectrometry [J]. J Chromatography A, 2006, 1103: [16],,, [J]., 2012, 33(06): Lu Y, Qu Y, Feng N, et al. Rapid Screening of 45 industrial dyes in foods by ultra performance liquid chromatography-tandem quadrupole mass spectrometry [J]. Food Sci, 2012, 33(06): [17],,,. - 6 [J]., 2011, 11(39): Cao P, Qiao XG, Lou XS, et al. Simultaneous determination of 6 industrial dyes in foods by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry [J]. Chin J Anal Chem, 2011, 11(39): [18],,,. -UPLC [J]., 2010, 31(24): Hou XL, Sun YJ, Wu GJ, et al. Use of solid-phase dispersine and ultra performance liquid chromatography for determination of para red and sudan- in egg yolk. [J]. Food Sci, 2010, 31(24): [19] Calbiani F, CareriM, Elviri L, et al. Development and in-house validation of a liquid chromatography-electrospray tandem mass spectrometry method for the simultaneous determination of sudanⅠ, sudanⅡ, sudan Ⅲ and sudan Ⅳ in hot chilli products [J]. J Chromatogr A, 2004, 1042: [20] Calbiani F, Careri M, Elviri L, et al. Accuratemass measurements for the confirmation of sudan azo-dyes in hot chilli products by capillary liquid chromatography-electrospray tandem quadrupoleorthogonal-acceleration time of flight mass spectrometry [J]. J Chromatogr A, 2004, 1058: [21] Zhu Y, Zhao B, Xiao R, et al. Simultaneous determination of 14 oil-soluble synthetic dyes in chilli products by high performance liquid chromatography with a gel permeation chromatography clean-up procedure [J]. Food Chem, 2014, 145(15): 作者简介 ( 责任编辑 : 杨翠娜 ) 路杨, 主管技师, 主要研究方向为食品检测技术 lyxyx00357@163.com 常凤启, 主任技师, 主要研究方向为食品安全与卫生检验 yanglixin241@163.com

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 蔡伟江 *, 邓鹏飞, 刘光兰, 李丹 (, 519040) 摘要 : 目的, 方法 (4.6 mm 250 mm, 5.0 μm) ; : : : =70: 16: 14(V:V:V),, : 1.0 ml/min; : 40 ; : 10

Microsoft Word 路 杨-二校 647

Microsoft Word 路杨-二校 647