摘要
目的建立高效液相色谱法检测肉及肉制品中甲醛含量的分析方法。方法用水蒸气蒸馏法提取,2,4-二硝基苯肼衍生化。优化蒸馏体积、最佳衍生条件。以甲醇和水为流动相、流速0.5mL/min、检测波长338nm的高效液相色谱条件进行测定。结果最终确定蒸馏体积为300mL,最佳衍生条件为55℃,30min。该方法在0~20mg/L浓度范围内线性关系良好(r2=0.9994),检出限0.1mg/kg,定量限为0.35mg/kg。在5、10、30mg/kg3个水平加标,测得的加标回收率为97.4%~107.8%,相对标准偏差(relative standard deviation,RSD)为3.77%~5.13%。结论用建立的方法对市售产品进行检测分析,结果可以满足肉及肉制品的检测需求。
Objective To establish a rapid and accurate method for determination of formaldehyde in meat and meat products by high performance liquid chromatography. Methods The formaldehyde in the sample was extracted by steam distillation, and derived by 2,4-dinitrophenylhydrazine. Distillation volume and derived conditions were optimized. The mobile phase was methanol and water, and flow rate was 0.5 mL/min. Detection wavelength was 338 nm in the conditions of high performance liquid chromatography. Results The distillation volume was determined to be 300 mL, and the optimal derivation conditions were 55 ℃ and 30 min. This method had a good linear relationship in the concentration range of 0-20 mg/L, with correlation coefficients(r 2 ) more than 0.9994. The limit of detection (LOD) was 0.1 mg/kg and the limit of quantification (LOQ) was 0.35 mg/kg. The average recoveries at 3 spiked concentration levels were 97.4%-107.8%, with the relative standard deviations (RSDs) were 3.77%-5.13%. Conclusion The established method is used to test and analyze the commercial products, and the results could meet the requirements of meat and meat products.
作者
吕青骎
滕爽
陈周耀
徐幸莲
王玮
LV Qing-Qin;TENG Shuang;CHEN Zhou-Yao;XU Xing-Lian;WANG Wei(College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China;Supervision, Inspection and Testing Center for Quality of Meat-Products, Ministry of Agriculture, Nanjing Agricultural University, Nanjing 210095, China)
出处
《食品安全质量检测学报》
CAS
2019年第11期3298-3303,共6页
Journal of Food Safety and Quality
基金
国家重点研发计划资助项目(2016YFF0201804)~~
关键词
甲醛
肉及肉制品
高效液相色谱法
formaldehyde
meat and meat products
high performance liquid chromatography
作者简介
吕青骎,助理实验师,主要研究方向为食品质量安全检测与控制。E-mail:f2014021@njau.edu.cn;通讯作者:王玮,博士,副教授,研究方向为食品质量安全控制。E-mail:wangwei821220@njau.edu.cn.
