摘要
建立并优化了聚能式脉冲超声-高效液相色谱-蒸发光散射测定概念鸡蛋中磷脂酰胆碱的分析方法。以正己烷-异丙醇-0.1%乙酸(8︰8︰1,体积比)为提取剂,在单因素试验基础上,以超声功率比、全程时间和液料比为影响因素,通过Box-Benhnken响应面优化法,确定磷脂酰胆碱的最佳提取条件:超声功率比40%,全程时间4.0 min,液料比15︰1(mL/g)。色谱柱为硅胶柱(4.6 mm×250 mm,5μm),流动相为正己烷-异丙醇-水-乙酸-三乙胺(2︰74︰24︰1.5︰0.08,体积比),流速为1.0 mL/min。蒸发光散射检测器漂移管温度为100℃,载气为氮气,流速为2.0L/min。磷脂酰胆碱在30~360 mg/L范围内呈良好线性关系,相关系数为0.9999。当加标量为1.722×10~3~8.630×10~3mg/kg时,回收率为95.8%~103.0%。方法精密度为2.53%,检出限为50 mg/kg。采用该方法对36种概念鸡蛋进行测定,结果表明该方法操作简便,快速,准确和重现性好,可满足实验要求。
A new method for the determination of phosphatidylcholine in conceptual eggs by energy-gathered pulsed ultrasonic-high performance liquid chromatography(HPLC)coupled with evaporative light scattering detection(ELSD)was developed.The sample was extracted with hexane-isopropanol-0.1%acetic acid(8︰8︰1,volume ratio)by energy-gathered pulsed ultrasonic.Based on one-factor analysis,Box-Benhnken response surface methodology(RSM)was employed to optimize extraction conditions,including ultrasonic power ratio,full work time and ratio of solvent to solid.The results showed that the optimal conditions were ultrasonic power ratio of 40%,full work time of 4.0 min and ratio of solvent to solid of 15︰1(mL/g).HPLC separation was performed on a silica gel column(4.6 mm×250 mm,5μm),and the mobile phase was hexane-isopropanol-water-acetic acid-triethylamine(2︰74︰24︰1.5︰0.08,volume ratio)at a flow rate of 1.0 mL/min.The ELSD parameters were as follows:drift tube temperature of 100℃,nebulizing gas(N2)flow rate of 2.0 L/min,respectively.PC showed good linearity in the concentration ranges of 30-360 mg/L,with the correlation coefficient of 0.9999.When the spiked concentration was between 1.722×103 and 8.630×103 mg/kg,the recoveries were between 95.8%and 103.0%.The relative standard deviations were 2.53%and the limit of detection was 50 mg/kg.The method was applied in the determination of 36 kinds of conceptual eggs.The results showed that this method was convenience,fast,accuracy and good repeatability,which could meet the determination of PC in conceptual eggs.
作者
陈兴
张娟
张军慧
CHEN Xing;ZHANG Juan;ZHANG Junhui(CCIC Central Plains Agricultural Products&Food Testing Co.,Ltd.,Zhengzhou 450000)
出处
《食品工业》
CAS
北大核心
2020年第6期314-318,共5页
The Food Industry
