摘要
使用超声萃取-反相高效液相色谱(HPLC)技术,建立同时分离和检测食物中苯甲酸、山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯6种防腐剂的方法。水-甲醇(5:95,V/V)作为提取溶剂进行超声萃取,采用Supelco Discovery C18反相色谱柱,流动相为乙腈-乙酸铵缓冲溶液(pH4.4)进行梯度洗脱,在1ml/min的流速和254nm的检测波长下14min内6种防腐剂得到良好分离。6种防腐剂线性范围从5μg/ml到100μg/ml,相关系数(r)为0.9997～1.0000。方法的平均回收率为90.1%～106.3%,精密度和稳定性的RSD分别为0.58%～1.79%、0.15%～1.65%,检出限的范围为0.012～0.43μg/ml。本方法的预处理过程简便、快速,应用于30种进出口食品中防腐剂的分析检测,检测结果灵敏、可靠。
An ultrasonic extraction-reversed phased HPLC method was developed for the simultaneous separation and determination of 6 common preservatives such as benzoic acid, sorbic acid, methylparaben, ethyl P-hydroxybenzoate, nipasol and butyl P-hydroxybenzoate. Samples were extracted with the mixture of water and methanol （5：95, V/V） in ultrasonic field. The gradient elution was carded out on a Supelco Discovery C18 column, with an initial mobile phase of acetonitrile-acetate buffer （pH 4.4） and at the flow rate of 1.0 ml/min. The detector wavelength was set at 254 nm. Under these conditions, the separation of the 6 components was achieved within 14 min. The linear ranges for the determination 6 preservatives by this method were from 5 to 100μg/ml with a correlation coefficient （r） of 0.9997-1.000, and the limits of detection were 0.012-0.43/ag/ml. The average recoveries for the 6 preservatives in sample spiked at three levels （10, 50 and 100μg/g） were 90.1% - 106.3% （n=3）. The RSDs of precision and stability were 0.58% - 1.79% （n = 5） and 0.15% - 1.65%, respectively. Finally, this method was applied to analysis of these preservatives in 30 different imported and exported food samples. Altogether, the pre-treatment procedure of the developed method is simple and rapid, and the result is sensitive and accurate.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2009年第12期198-201,共4页
Food Science
关键词
RP-HPLC
超声萃取
同时测定
防腐剂
食品
RP-HPLC
ultrasonic extraction
simultaneous determination
preservative
foods
