7 6 Vol. 7 No. 6 2016 6 Journal of Food Safety and Quality Jun., 2016 戚美静 1*, 杨冀艳 1, 朱昌磊 2, 姚凌峰 1, 洪春苗 (1. ( ), 300457; 2., 266101) 1 摘要 : 目的 2(chrysoidine G, CDG) 21(orange G, AOG) 22(astrazon orange R, AOR) 方法 : : (60:40:0.5, V:V:V) 25 30 min, 0.02 mol/l (ph 5), Agilent XDB C 18, 449 nm CDG, 485 nm AOG AOR, 结果 3 0.01~0.2 mg/l, 80.0%~94.0%, 2%(n=6), 0.1 mg/kg 结论, 关键词 : ; ; ; Determination of basic orange dyes in food by high performance liquid chromatography QI Mei-Jing 1*, YANG Ji-Yan 1, ZHU Chang-Lei 2, YAO Ling-Feng 1, HONG Chun-Miao 1 (1. SGS-CSTC Standards Technical Services (Tianjin) Co., Ltd., Tianjin 300457, China; 2. SGS-CSTC Standards Technical Services Co., Ltd., Qingdao Branch, Qingdao 266101, China) ABSTRACT: Objective To establish a method for determination of 3 kinds of basic orange dyes by high performance liquid chromatography(hplc), including chrysoidine G (CDG), astrazon orange G (AOG) and astrazon orange R (AOR). Methods Samples were extracted with ultrasonic for 30 min by acetonitrile: water: ammonium hydroxide (60:40:0.5, V:V:V) at 25. Ammonium acetate (0.02 mol/l, ph=5) and acetonitrile were used as mobile phase for gradient elution, an Agilent XDB C 18 column was used for separation, and diode array detector was used for the determination of CDG at 449 nm and AOG and AOR at 485 nm with external standard method for quantification. Results Three kinds of basic orange dyes had good linear relationships in the range of 0.01~0.2 mg/l. The average recoveries were 80%~94% and the relative standard deviations were less than 2% (n=6). The detection limits of the method were 0.1 mg/kg. Conclusion The method is simple and accurate, which is suitable for the determination of basic orange dyes in yuba, dry chili and chili oil. KEY WORDS: high performance liquid chromatography; basic orange dyes; food; dyes 1 引言, [1], [2], [3] * 通讯作者 :,, E-mail: qmj07huayi@126.com *Corresponding author: QI Mei-Jing, Assistant Engineer, SGS-CSTC Standards Technical Services (Tianjin) Co.,Ltd., Tianjin 300457, China. E-mail: qmj07huayi@126.com
2524 7,,,,, 3, 2(chrysoidine G, CDG) 21(orange G, AOG) 22(astrazon orange R, AOR) (high performance liquid chromatography, HPLC) - [4-14],,, GB/T 23496-2009 [15],, 3,, 2 材料与方法 2.1 材料,, 2.2 仪器与试剂 (, ); (, ); 2 21 22( >99%, Sigma ) Agilent 1260 ( ); (Eppendorf ); ( ); (CREST ); ( ) 2.3 实验方法 2.3.1 标准溶液的配制 1.0 g/l : 2 21 10 mg, 10 ml; 10 mg/l : 100 μl, 10 ml; :, 0.01 0.02 0.05 0.1 0.2 mg/l, : : : =60:40:0.5(V:V:V), 2.3.2 样品前处理 (1) 2.5 g, 25 ml, 30 min, 4000 r/min 10 min, 0.45 μm, (2) 2.5 g, 10 ml, 25 ml, 30 min, 4000 r/min 10 min, 0.45 μm, 2.3.3 仪器条件 Agilent XDB C 18 (4.6 mm 150 mm, 5 μm); : A: 0.02 mol/l ( ph 5.0); B: ; : 1.0 ml/min; : 30 ; : 2: 449 nm; 21 22: 485 nm : 100 μl : ; 1 3 结果与分析 3.1 流动相 ph 的选择 A ph, C 18, 21 2, ( 1~2) ph 21, 21 2 ( 3~4), 22 ; ph C 18,, ph ph 5, 3.2 提取试剂的选择,,, GB/T 23496-2009 [15] 3 65% ;, 2 2, 2 3, 2.3.2, 2 2,,, 0.5% -60%, 0.5% - 60% 3.3 提取温度和时间的选择 25 50 ( 5), 30 min,, ; 25, 10 30 60 min ( 6),, 30 min 60 min,, 25 30 min, 50,
6, : 2525 Table 1 表 1 流动相梯度洗脱程序 Gradient program of mobile phase /min 0 3 16 18 18.1 20 A/% 60 60 5 5 60 60 B/% 40 40 95 95 40 40 Fig. 1 1 2 ( 449 nm) Chromatogram of standard CDG (wavelength of 449 nm) 2 21 22 ( 485nm) Fig. 2 Chromatogram of standard AOG and AOR (wavelength of 485 nm)
2526 7 Fig. 3 3 2 ( 449 nm, ph=5) Chromatogram of standard CDG (wavelength of 449 nm, ph=5) 4 21 22 ( 485 nm, ph=5) Fig.4 Chromatogram of standard AOG and AOR (wavelength of 485 nm, ph=5) 表 2 不同提取剂提取 3 种基质中碱性橙 2 的含量结果 (n=3) Table 2 Results of CDG in 3 kinds of matrix extracted by different extracting agents (n=3) : mg/kg 60% 0.5% -60% 0.5% -60% 0.5% -60% + 8.2 60.5 10.5 76.5 / 4.3 40.6 0 45.8 / 11.5 5.2 0 63.6 94.8
6, : 2527 Fig. 5 5 Effect of extraction temperature on recovery rate 6 Fig.6 Effect of ultrasonic time on recovery rate Table 3 表 3 线性回归方程 相关系数及检出限 Linear regression equations, correlation coefficients and limits of detection (mg/kg) 21 Y=2339.245X-1.8824 0.99994 0.1 2 Y=1228.436X-0.4789 0.99993 0.1 22 Y=4549.030X-1.2589 0.99990 0.1 表 4 回收率结果 (n=6) Table 4 Results of recoveries (n=6) (0.01 mg/l) (0.01 mg/l) (%) RSD/% 21 0.01 0.0090 90.0 1.5 2 0.01 0.0094 94.0 1.8 22 0.01 0.0086 86.0 0.9 21 0.01 0.0090 90.0 1.6 2 0.01 0.0080 80.0 1.2 22 0.01 0.0082 82.0 0.89 21 0.01 0.0085 85.0 1.4 2 0.01 0.0081 81.0 1.2 22 0.01 0.0081 81.0 0.87 3.4 线性关系及检出限 2 21 22 3, 0.01~0.2 mg/l ; 3(S/N=3), 3 3.5 回收率实验 0,, 4 4 结论 3, 3 0.01~0.2 mg/l, 80%~94%, 参考文献 [1]. : [M]. :, 2004. He HL. Fine chemical product manuals: dye [M]. Beijing: Chemical Industry Press, 2004. [2]. [M]. :, 1990. Chinese academy of sciences institute of labor hygiene and occupational
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