Microsoft Word 黄志强-二校回

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1 6 5 Vol. 6 No Journal of Food Safety and Quality May., 2015 黄志强 *, 王飞, 俞文妍, 杨献青 (, ) 摘要 : 目的 7 ( ) -(solid-phase extraction-high performance liquid chromatography, SPE-HPLC) 方法, Anpelclean PA SPE,, 20 mmol/l, Waters XBridge C 18, 结果 ~10.0 µg/ml (r ), mg/kg 74.3%~97.5%, RSD 0.47%~4.80% 0.02~0.10 mg/kg, 0.06~0.30 mg/kg 结论,,,, 7 关键词 : ; ; ; Determination of 7 kinds of synthetic pigments in preserved fruits by solid-phase extraction-high performance liquid chromatography HUANG Zhi-Qiang *, WANG Fei, YU Wen-Yan, YANG Xian-Qing (Jiande Center for Disease Control and Prevention, Jiande , China) ABSTRACT: Objective To establish a method for simultaneous determination of 7 kinds of synthetic pigments (lemon yellow, amaranth, ponceau 4r, sunset yellow, coomassie brilliant blue, allura red and erythrosine) in preserved fruits with solid-phase extraction-high performance liquid chromatography (SPE-HPLC). Methods The homogenized samples were extracted by water, purified by Anpelclean PA- SPE column, and adjusted to constant volume after nitrogen blowing. HPLC analysis was conducted using methanol and 20 mmol/l ammonium acetate as mobile phase with a xbridge-c 18 column from Waters company for gradient elution and separation. Specific wavelengths were applied for quantitative detection of the synthetic pigments in the samples. Results There was a good linearity between peak areas and concentrations of 7 kinds of synthetic pigments in the concentration range of 0.50~10.0 μg/ml (r ). The recovery rates fell in the scope of 74.3%~97.5% and RSDs ranged from 0.47% to 4.80% under the standard addition levels of 0.5, 2.5 and 5.0 mg/kg. The detection limits were between 0.02 and 0.10 mg/kg and the quantification limits between 0.06 and mg/kg. Conclusion The method has high sensitivity, good separation effect, good precision and high accuracy, thus, it s suitable for the simultaneous determination of 7 kinds of common fruit pigments in * 通讯作者 :,, hzqwsjy@163.com *Corresponding author: HUANG Zhi-Qiang, Technician, Jiande Center of Disease Control and Prevention, No.66 Kang'an Road, Xin An River Street, Jiande , China. hzqwsjy@163.com

2 preserved fruits. KEY WORDS: solid-phase extraction; preserved fruits; synthetic pigments; high performance liquid chromatography 1 引言,,,,, R-N=N-Rc, [1],,, [2] GB [3] [4-10] - [11],, -,, [12],, 7,,, 2 材料与方法 2.1 仪器与试剂 Waters E ( ); KL512J ( ); Delta320 ph (- ); Anpelclean PA (300 mg, 6 ml)(); GM-1.0A ( ); Mediwax ( Mediwax ) (0.500 mg/ml, ); (1.00 mg/ml, ) (, ); (, ); (, ); (, ); (, ); (0.02 mol/l): 1.54 g, 1000 ml,, 0.45 μm - -(7:2:1, V:V:V) : 70 ml 20 ml 10 ml, (ph=6.0):, ph 实验方法样品前处理 5.00 g,, 30 ml, min,, 3, ph ph 6 : ph=6.0 :, : 5 ml ph=6.0, 5 ml - (3:2, V:V), ( 3~5 )( ph ), : - - (7:2:1, V:V:V),, : 60, 1~2 ml, ph, 5 ml, 0.22 μm, [13] 色谱条件 : Waters XBridge C 18 (4.6 mm 250 mm 5 μm), : A, B (0.02 mol/l) 1 2 Table 1 表 1 流动相梯度洗脱表 Table of mobile phase gradient elution (min) A (%) B (%) : /

3 5, : 表 2 波长设置表 Table 2 Table of setting wavelength (min) (nm) 0~ ~ ~ ~ ~ ~ ~ ~ 标准曲线的配制 5.0 ml 2.5 ml 50.0 ml,, 50 μg/ml ml 50.0 ml,, μg/ml 2.2.2,, 3 结果与讨论 3.1 样品前处理条件的确定,,, [14] GB/T [15],, ph 6, [13,15,16] 3.2 色谱分离条件的确定 GB/T [15] 254 nm,,, GB/T [17] : 428 nm, 521 nm, 509 nm, 483 nm, 507 nm, 625 nm, 529 nm GB/T [15] GB/T [17],,,, 1, 2.1 min, 2, 3.3 标准曲线与检出限 0.50~10.0 µg/ml, 7, 3, 10 1 Fig. 1 Standard chromatogram

4 1944 6, 3 GB/T [15] ~1.04 mg/kg, 0.02~0.10 mg/kg, GB [3] ~0.1 g/kg, 0.06~0.30 mg/kg, 3.4 方法的精密度和加标回收率 mg/kg 7, 2.2.2,, 3, 74.3%~97.5%, 91.8%, RSD 0.47%~4.80%3 75.6%~96.8%, 91.0%, RSD 0.61%~4.60% 结论 GB/T GB/T , mg/kg 74.3%~97.5%, RSD 0.47%~4.80%, 0.02~0.10 mg/kg Fig. 2 2 Chromatogram of lover plum sample Table 3 表 3 7 种合成色素标准曲线回归方程线性系数检出限和定量限 Standard curves, regression equations, linear coefficients, detection limits and quantification limits of 7 kinds of synthetic pigments r 2 (mg/kg) (mg/kg) Y= X Y= X Y= X Y= X Y= X Y= X Y= X

5 5, : Fig. 3 3 Chromatogram of preserved mango samples Fig. 4 4 (0.5 mg/kg) Chromatogram of spiked preserved mango sample (0.5 mg/kg) 表 4 7 种色素加标回收率结果 (n=6) Table 4 The recovery rates of 7 kinds of pigments (n=6) (mg/kg) (%) RSD(%) (%) RSD(%)

6 续表 4 (mg/kg) (%) RSD(%) (%) RSD(%) , 0.06~0.30 mg/kg,,,,,,, 7 参考文献 [1] Collier SW, Storm JE, Bronaugh RL, Reduction of azodycs during invitro percutaneous absorption [J]. Toxicol Appl Pharmacol, 1993, (118): [2],,. - [J]., 2013, 23(7): Wen J, Sun DH, Hu XK. Simultaneous determination of 7 kinds of synthetic pigments in foods by SPE-HPLC [J]. Chin J Health Lab Technol, 2013, 23(7): [3] GB [S]. GB National food safety standards-hygienic standards for uses of food additives [S]. [4],,,. 16 [J]., 2011, 30(6): Liu Y, Yin Z, Zou XX, et al. Determination of 16 kinds of food additives in preserved fruits by high performance liquid chromatography [J]. J Instrum Anal, 2011, 30(6): [5],,. HPLC 8 [J]., 2013, 23(1): Hua YY, Lin J, Lin HL. Determination of synthetic pigment in health foods by HPLC [J]. Chin J Health Lab Technol, 2013, 23(1): [6],,,. 8 [J]., 2014, 5(12): Kong C, Shen XS, Yu HJ, et al. Determination of 8 synthetic food colorants in protein-rich samples with high performance liquid chromatography [J]. J Food Saf Qual, 2014, 5(12): [7],,,. 7 [J]., 2014, 30(4): Yan B, Hu HS, Zhang YW, et al. Determination of 7 kinds of synthetic pigments in foods by ultra performance liquid chromatography [J]. J Anal Sci, 2014, 30(4): [8],,,. 7 [J]., 2014, 21(6): Zhou R, Mou RX, Xu P, et al. Determination of 7 kinds of synthetic pigments in food by HPLC [J]. Cereal Food Ind, 2014, 21(6):

7 5, : [9],,,. [J]., 2014, 5(12): Hao PF, Gong P, Liu L, et al. Determination of sunset yellow, carmine and allura red in cooked meat products by high performance liquid chromatography [J]. J Food Saf Qual, 2014, 5(12): [10],,,. 19 [J]., 2014, 5(11): Chen PJ, Zhang Y, Xiao F, et al. Determination of 19 kinds of food additives in candies, preserves and beverages by high performance liquid chromatography [J]. J Food Saf Qual, 2014, 5(11): [11],,,. [J]., 2007, 128(10): Xing XH, Yin WH, Han CJ, et al. Method for determination of synthetic colors in preserved fruit [J]. Food Res Dev, 2007, 128(10): [12]. / 9 [J]., 2014, 23(5):1 5. Yang WQ. Determination of 9 kinds of synthetic colorants in food by auto-solid phase extraction/ultra-performance liquid chromatography tandem mass spectrometry [J]. Fujian Anal Test, 2014, 23(5): 1 5. [13],,,. - 4 [J]., 2014, (6): Xiao L, Yu ZF, Xue F, et al. Simultaneous determination of four synthetic colorants in dried shrimps by polyamide cartridge and HPLC [J]. Chin Food Addit, 2014, (6): [14]. [J]., 2010, 28(3): Zhang JY. Determination of synthetic colour in glazed fruit by high performance liquid chromatography [J]. J Kaili Univ, 2010, 28(3): [15] GB/T [S]. GB/T Determination of synthetic colour in foods [S]. [16],,. - [J]., 2014, 24(22): Chi QC, Liu C, Yan C. Simultaneous determination of indigo and erythrosine in foods with solid-phase extraction-high performance liquid chromatography [J]. Chin J Health Lab Technol, 2014, 24(22): [17] GB/T [S]. GB/T Determination of synthetic colour in fruit tins-high performance liquid chromatography [S]. 作者简介 ( 责任编辑 : 卢忆 ) 黄志强, 技师, 主要研究方向为食品理化检验 hzqwsjy@163.com

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0.