HPLC Determination of Preservatives in Food of Various Matrixes
摘 要
取固体样品(如糕点、肉肠等) 2.000 g,或液态样品(如饮料等) 10.00 mL,加少量水稀释后,加入220 g·L-1乙酸锌和106 g·L-1亚铁氰化钾溶液各2 mL沉淀蛋白质并离心除去;取半固体样品(如果冻等) 2.000 g,加水稀释后用氨水(1+1)溶液调节其酸度至pH 7~8,上述3种样品溶液均分别用水定容至25.0 mL。所得溶液进行高效液相色谱分离,以TSK Eclipse XDB-C18色谱柱为固定相,和pH 5.0的甲醇-三乙胺缓冲溶液(1+9)为流动相。苯甲酸和山梨酸的质量浓度均在0.1~10.0 mg·L-1内与峰面积呈线性关系,检出限(3S/N)分别为1.8,1.2 mg·kg-1。按标准加入法在3个浓度水平上进行回收试验,回收率在90%~97%之间,测定值的相对标准偏差(n=6)均小于10%。
Abstract
The solid sample, e.g. cake, sausage and etc., (2.000 g) or liquid sample, e.g., drinks etc. (10.00 mL) was taken and diluted with some water. 2 mL of 220 g·L-1 zinc acetate solution and 2 mL of 106 g·L-1 potassium ferrocyanide solution were added to precipitate protein and to remove it by centrifuge. In case of semi-solid sample, e.g., jelly, 2.000 g were taken and diluted with water. The acidity was adjusted to pH 7 to 8 with ammonia (1+1) solution. The sample solution described above was made up to 25.0 mL with water, and separated by HPLC using TSK Eclipse XDB-C18 column as stationary phase and mixed solution of methanol and triethylamin (1+9) (pH 5.0) as mobile phase. Linear relationships between values of peak area and mass concentration of benzoic acid and sorbic acid were found in the same range of 0.1-10.0 mg·L-1, with detection limits (3S/N) of 1.8, 1.2 mg·kg-1, respectively. Test for recovery was made by standard addition method at 3 concentration levels, giving results in the range of 90%-97%, with RSDs (n=6) less than 10%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201704016
所属栏目 工作简报
基金项目
收稿日期 2016/3/17
修改稿日期
网络出版日期
作者单位点击查看
联系人作者刘谦(chemliuq@163.com)
备注刘晓慧(1980-),女,河北保定人,博士,研究方向为食品中微生物的检测。
引用该论文: LIU Xiao-hui,LIU Qian,WU Xin-xin,GUO Li-qiang,LIU Ping. HPLC Determination of Preservatives in Food of Various Matrixes[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(4): 447~450
刘晓慧,刘谦,吴新欣,郭力强,刘萍. 高效液相色谱法测定不同基质的食品中防腐剂含量[J]. 理化检验-化学分册, 2017, 53(4): 447~450
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参考文献
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【5】符传武,覃子龙.RP-HPLC法测定食用动物油脂中苯甲酸与山梨酸的含量[J].中国酿造, 2014,33(1):143-146.
【6】杨凤艳,孙玉娟.高效液相色谱法测定腐乳中的苯甲酸、山梨酸[J].中国卫生检验杂志, 2010,20(8):1873-1874.
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