摘要
建立高效液相色谱串联质谱法测定红心鸭蛋中紫杉紫素含量的方法。样品经乙腈提取,浓缩后用正己烷脱脂。采用Shim-pack XR-ODSⅢ(1.6μm, 2.0 mm×75 mm)色谱柱分离,以5 mmol/L乙酸铵和乙腈作为流动相进行梯度洗脱,流速0.3 mL/min。采用电喷雾电离源、正离子模式,在多反应监测模式进行扫描。紫杉紫素在5.0~100.0 ng/mL范围内线性相关系数为0.999 7,检出限为10μg/kg;在3个浓度水平(10~200μg/kg)的加标回收率在86.7%~94.5%,相对标准偏差(δRSD)在1.62%~3.45%(n=6)。该方法准确、可靠,适用于红心鸭蛋中紫杉紫素含量的检测。
A high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of rhodoxanthin in red yolk of duck’s eggs. Samples were extracted with acetonitrile. After concentrated, the acetonitrile phase was defatted by hexane. Chromatographic separation was performed on a Shim-pack XR-ODS Ⅲ(1.6 μm, 2.0 mm×75 mm) column with acetonitrile-5 mmol/L ammonium acetate as mobile phase by gradient elution. The flowrate was 0.3 mL/min. The detection was performed using an electrospray ionization(ESI)-mass spectrometer with multiple reaction monitoring(MRM) in positive mode. Rhodoxanthin displayed a linear relationship in the range of 5.0-100 μg/L with correlation coefficients of 0.999 7. The detection limits of rhodoxanthin were 10 μg/kg. The recoveries of rhodoxanthin at 3 concentration levels(10-200 μg/kg) were within the range of 86.7%-94.5%, and the relative standard deviation(δRSD) was 1.62%-3.45%(n=6). The results showed that method was accurate and reliable, and it was suitable for the determination of rhodoxanthin in red yolk of duck’s eggs.
作者
蔡翔宇
欧玉玲
陈晓兰
梁宇
CAI Xiangyu;OU Yuling;CHEN Xiaolan;LIANG Yu(Technology Center of Nanning Customs,Nanning 530021;Guilin Customs,Guilin 541000)
出处
《食品工业》
CAS
2021年第4期433-436,共4页
The Food Industry
基金
海关总署科技计划项目(2017IK040)。
关键词
高效液相色谱串联质谱
红心鸭蛋
紫杉紫素
high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)
red yolk of duck’s eggs
rhodoxanthin
