摘要
基于目标化合物的弱酸性及小麦粉基质的特点,通过对不同提取剂、流动相组成、梯度条件及色谱柱的选择及优化,建立了高效液相色谱-二极管阵列检测器(HPLC-PDA)测定小麦粉中苯甲羟肟酸的分析方法。样品中的苯甲羟肟酸采用甲醇提取,无需净化,以甲醇-磷酸盐(p H 3.7)为流动相,Waters Xbridge C18色谱柱完成了对目标物及特定干扰物的完全分离,高效液相色谱-二极管阵列检测器检测,外标法定量。该方法在0.1~10μg/mL范围内线性关系系数(r^(2))大于0.999;方法检出限为0.1 mg/kg,定量限为0.5 mg/kg;在定量限(LOQ),2 LOQ和10 LOQ 3个添加水平下重复测定6次的回收率为93.7%~102.7%,相对标准偏差(RSD)为1.1%~3.8%。该方法适用于小麦粉中苯甲羟肟酸的测定。
Based on the weak acid properties of the target compounds and the characteristics of wheat flour matrix,an easy extraction procedure coupled with high performance liquid chromatography-photodiode array method(HPLCPDA)was established for the determination of benzohydroxamic acid in flour.The selection and optimization of different extraction agents,mobile phase composition,gradient conditions and chromatographic columns were studied.Benzyl hydroxamic acid in the sample was extracted by methanol without cleanup.The target and specific interferents were completely separated on Waters Xbridge C18 column with methanol-phosphate(p H 3.7)as mobile phase,and detected by high performance liquid chromatography-diode array detector(HPLC-PDA).The linear correlation coefficient(r^(2))is more than 0.999 in the range of 0.1-10μg/m L.The limit of detection(LOD)and the limit of quantification(LOQ)were 0.1 mg/kg and 0.5 mg/kg,respectively.The average recoveries were in the range of93.7%-102.7%with the relative standard deviation(RSDs)of 1.1%-3.8%at three spiked levels of LOQ,2 LOQ and 10 LOQ.The method is suitable for the analysis of benzohydroxamic acid in flour.
作者
于文江
周传静
尹丽丽
薛霞
程志
张喜琦
郑红
刘艳明
YU Wenjiang;ZHOU Chuanjing;YIN Lili;XUE Xia;CHENG Zhi;ZHANG Xiqi;ZHENG Hong;LIU Yanming(Shandong Institute for Food and Drug Control,Shandong Institute for Food and Drug Safety Testing Engineering Technology Research Center,Jinan 250101)
出处
《分析试验室》
CAS
CSCD
北大核心
2021年第4期429-432,共4页
Chinese Journal of Analysis Laboratory
基金
山东省重点研发计划(2019YYSP020)
食品安全关键技术研发重点专项(2017YFC1601600)资助。
关键词
苯甲羟肟酸
小麦粉
高效液相色谱法
二极管阵列检测器
benzohydroxamic acid(b-acid)
flour
high performance liquid chromatography(HPLC)
photodiodearray detection(PDA)
