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扉创趣籍
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1 7 7 Vol. 7 No Journal of Food Safety and Quality Jul., 2016 * 唐穂平 (, ) 摘要 : 目的方法, 2, 4- - (1:1, V:V) 60 1 h,, ODS-C 18, - (70:30, V:V), 365 nm, 结果 0~10 mg/l, , 0.5 mg/kg mg/kg, 88.2%~95.3%, RSD 0.75%~1.82% 9, 6, 1.51~64.04 mg/kg 结论, 关键词 : Determination of formaldehyde in aquatic products by high performance liquid chromatography with precolumn derivatization TANG Sui-Ping * (Guangdong Testing Institute for Product Quality Supervision, Foshan , China) ABSTRACT: Objective To establish a method for the determination of formaldehyde in aquatic products by high performance liquid chromatography with precolumn derivatization. Methods After homogenation and homogeneity, samples were derivatized with 2, 4-dinitrobenzene hydrazine derivative-sodium acetate buffer (1:1, V:V) at 60 for 1 h. After ice bath cooling, the derivatives were determined by high performance liquid chromatography (HPLC) using ODS-C 18 column for separation with methanol and water (70:30, V:V) as the mobile phase for isocratic elution, and then detected by diode array detector at 365 nm wavelength with external standard method for quantification. Results Formaldehyde had a good linear relationship in the range of 0~10 mg/l with correlation coefficient of , and the limit of detection was 0.5 mg/kg. The recoveries spiked at 3 levels of 1.0, 5.0 and 20.0 mg/kg were 88.2%~95.3% with RSD of 0.75% ~ 1.82%. Nine aquatic products were determined, and 6 samples were detected, the content range of formaldehyde were 1.51~64.04 mg/kg. Conclusion The method is simple, sensitive and accurate, which can be applied for the analysis of formaldehyde in aquatic products. KEY WORDS: formaldehyde; aquatic product; precolumn derivatization; high performance liquid chromatography * 通讯作者 :,,, Tang2068@126.com *Corresponding author: TANG Sui-Ping, Master, Engineer, Guangdong Testing Institute for Product Quality Supervision, Foshan , China. Tang2068@126.com

2 引言,,,, [1,2],,,,, [3], [4,5] (gas chromatograph, GC) [6-8] (high performance liquid chromatography, HPLC) [9-11],,,,,, [12-14] SC/T [15],,,,, 2.2 实验方法标准溶液的配制 1000 mg/l : 0.1 g( g) 100 ml, ; : mg/l 样品前处理 2 g( 0.01 g), 20 ml 2, 4- - (1:1, V:V), 2 min, 60, 1 h, 0.45 μm, 液相色谱条件 : ODS-C 18 (250 mm 4.6 mm, 5 µm); : 365 nm; : 20 µl; : 1.0 ml/min; : 40 ; : : (70:30, V:V) 3 结果与分析 3.1 衍生液溶剂的选择和 ph 值控制 2, 4-,,,, ph ( 1),, ph , ph 材料与方法 2.1 仪器与试剂 LC20A ( PDA, ); IKA ( IKA ); Sigma ( Sigma ); HGC ( ); THZ-100B ( ); Sigma ( Sigma ) (, 35%~40%, ); (, 99.9%, ); (, 99.0%, ); 2,4- (, 99.0%, ); ( 2.64 g,, 1.0 ml, 500 ml, ph 4.0); 1 ph Fig. 1 Effects of derivative ph on the extraction of formaldehyde 3.2 衍生温度和时间的比较, ( 2),, 60 ; min( 3),, 60 min, 60 1 h

3 7 穂 : 线性范围与检出限 5, mg/l,, X Y, ( 8), : Y=605.3X-55.2, r= S/N mg/kg Fig. 2 2 Effects of derivative temperature on the extraction of formaldehyde 3.5 回收率试验, mg/kg 6, 1 1, %~95.3%, RSD 0.75%~1.82%, 3.6 水产品及其制品中甲醛含量调查结果 3 Fig. 3 Effects of derivative time on the extraction of formaldehyde 3.3 样品谱图 2.2.3, 4~7,, 9,, ( 2),,,,, Fig. 4 4 Chromatogram of blank solution

4 Fig. 5 5 Chromatogram of standard solution Fig. 6 6 Chromatogram of sample solution Fig. 7 7 Chromatogram of spiked sample solution

5 7 穂 : 2935 Fig. 8 8 Standard curve of formaldehyde Table 1 表 1 不同样品不同添加浓度的回收率 (n=6) Recoveries of different samples with different concentrations (n=6) (mg/kg) (mg/kg) (%) RSD(%) 表 2 水产品及其制品中甲醛含量测得结果 (n=3) Table 2 Content of formaldehyde in aquatic products (n=3) (mg/kg), 50.12± ±1.12, 49.61± ±0.79, 64.04± ±1.42, 1.51± ±0.32,,, 36.11± ±0.23, 27.91± ±077,

6 2936 7,,,,, [16] ;,, (TMAO-ase),, 4 结论 2, 4- -, 60 1 h,,,, 参考文献 [1] Takigawa T, Horike T, Ohashi Y, et al. Were volatile organivc compounds the inducing factors for subjectivesymptoms of employees woorking in newly constructed hospitals [J]. Environ Toxicol, 2004, 19(4): [2] Nalivaiko E, DePasquale CG, Blessing WW. Electrocardiographic changes associated with the nasopharyngeal telex in conscious rabbits: vagosympathetic co-activation [J]. Auton Neurosci, 2003, 05(2): [3] Cole P, Axten C. Form aldehyde and leukemia: fill improbable causal relationship [J]. Nesul Toxicol Pharm, 2004, 40(2): [4],. [J]., 2014, 50(1): Li YC, Li JR. Research progress on endogenous formaldehyde in aquatic products [J]. Food Ferment Technol, 2014, 50(1): [5],,. [J]., 2004, 25(5): Zhao XZ, Sun JW, Yao L. Chemical analysis of trace formaldehyde in food research [J]. Food Ind Sci Technol, 2004, 25(5): [6],. - [J]., (2): Zhang HJ, Ember. Derivative - SPE coupled spectrophotometric method determination of formaldehyde and its application [J]. J Anal Sci, 2013, 29(2): [7],,,. [J]., 2012, 40 (3): Cao ZK, Jin CP, Ge PP, et al. Industrial formaldehyde gas chromatography analysis method to improve [J]. J Guangzhou Chem Ind, 2012, 40(3): [8] Kee CL, Lai CS, Ge XW, et al. Partial conversion of methanol to formaldehyde in the gas chromatography injection port and reactivity with amines [J]. J Chromatogr A, 2012, 1257(1257): [9],,. [J]., 2015, (6): Han DJ, Li Y, Liu HY. Research progress on endogenous formaldehyde in aquatic products [J]. J Food Saf Qual, 2015, (6): [10] Xu X, Su R, Zhao X, et al. Determination of formaldehyde in beverages using microwave-assisted derivatization and ionic liquid-based dispersive liquid-liquid microextraction followed by high-performance liquid chromatography [J]. Talanta, 2011, 85 (5): [11] Wang T, Gao XL, Tong J, et al. Determination of formaldehyde in beer based on cloud point extraction using 2, 4-dinitrophenylhydrazine as derivative reagent [J]. Food Chem, 2012, 131(4): [12],,,. [J]., 2008, 29(6): Gu XY, Bao ZD, Xu RN, et al. Derived gas chromatography for determination of formaldehyde in beer [J]. J Food Res Dev, 2008, 29(6): [13],,,. [J]., 2014, 35(6): Jiang YY, Li XP, Zou ZY, et al. Study on reaction characteristics of apple polyphenols and formaldehyde and its application in dried-seasoned squid processing [J]. Sci Technol Food Ind, 2014, 35(6): [14] Bianchi F, Careri M, Musci M, et al. Fish and food safety: determination of formaldehyde in12 fish species by SPME extraction and GC-MS analysis [J]. Food Chem, 2007, 100: [15] SC/T [S]. SC/T The determination of formaldehyde in aquatic products [S]. [16],,. [ J]., 2004, 10: Zhou QH, Peng K, Wang Y. New progress in determination of formaldehyde in foods and the comparison of various methods [J]. J Food Sci Technol, 2004, 10: 作者简介 ( 责任编辑 : 姚菲 ) 唐穗平, 硕士, 工程师, 主要研究方向为食品安全检测与研究 Tang2068@126.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.