摘要
目的:进行了乙醇替代甲醇作为提取剂和流动相的RP-HPLC法同时测定豆瓣酱中4种尼泊金酯的一测多评研究。方法:样品经乙醇提取,采用CAPCELL PAK C_(18)(4.6 mm×250 mm,5μm)色谱柱分离,以乙醇、水为流动相,以尼泊金甲酯为参考,建立了4种尼泊金酯类的定量模型。试验进行了流速、柱温及方法学、供试品溶液和色谱柱稳定性的考察。结果:试验表明因乙醇的黏度较甲醇大,柱温选择35℃、流速选择0.5 mL/min较为合适;校正因子分别为f_(乙/甲)=0.8721、f_(丙/甲)=0.8803、f_(丁/甲)=0.7103,且耐受性良好;4种尼泊金酯方法检出限在0.06~0.14 mg/kg之间;在5,10,40μg/kg三水平下的加标回收率及精密度分别为尼泊金甲酯85.4%~95.0%、2.7%~4.9%;尼泊金乙酯86.7%~95.0%、3.0%~3.7%;尼泊金丙酯85.2%~94.0%、2.7%~3.5%;尼泊金丁酯84.8%~96.1%、1.2%~3.7%。结论:该方法在确保测定数据准确的基础上,具有环境兼容性和经济性的特点,适用于豆瓣酱中4种尼泊金酯类的测定。
Objective:The QAMS study on simultaneous determination of four nipagin esters in bean paste by RP-HPLC with ethanol instead of methanol as the extractant and mobile phase is carried out.Methods:The samples are extracted by ethanol and separated by CAPCELL PAK C_(18)(4.6 mm×250 mm,5μm)chromatographic column,with ethanol and water as the mobile phases.The quantitative models of four nipagin esters are established with nipagin methyl paraben as the reference.The flow rate,column temperature,methodology,test solution and chromatographic column stability are investigated.Results:Because the viscosity of ethanol is higher than that of methanol,it is more appropriate to choose column temperature to be 35℃and flow rate to be 0.5 mL/min.The correction factors are f_(B/A)=0.8721,f_(C/A)=0.8803 and f_(D/A)=0.7103 respectively,and their tolerance is good.The method detection limits of the four nipagin esters are 0.06~0.14 mg/kg.The spiked recovery rate and precision at the three levels of 5,10,40μg/kg are nipagin methyl paraben 85.4%~95.0%,2.7%~4.9%;nipagin ethyl paraben 86.7%~95.0%,3.0%~3.7%;nipagin propyl paraben 85.2%~94.0%,2.7%~3.5%;nipagin butyl paraben 84.8%~96.1%,1.2%~3.7%respectively.Conclusion:On the basis of ensuring the accuracy of the measured data,this method has the characteristics of environmental compatibility and economy,and is suitable for the determination of four nipagin esters in bean paste.
作者
刘超
景赞
余敏灵
LIU Chao;JING Zan;YU Min-ling(Leshan Food and Drug Inspection and Testing Center,Leshan 614000,China)
出处
《中国调味品》
CAS
北大核心
2022年第10期169-172,共4页
China Condiment
基金
四川省市场监管系统科技计划项目(SCSJZ2022016)。
关键词
一测多评
尼泊金酯
乙醇替代甲醇
反向高效液相色谱法
quantitative analysis of multi-components by single marker(QAMS)
nipagin esters
ethanol instead of methanol
RP-HPLC
