摘要
目的:建立一种采用超高效液相色谱-串联质谱法检测核桃中井冈霉素残留的分析方法。方法:核桃样品经CH_(3)OH提取后,用HLB固相萃取柱净化,然后过C_(18)色谱柱分离。将获得的样品用CH_(3)OH-0.05%的ammonium acetate缓冲溶液的流动相进行梯度洗脱。采用UPLC-MS/MS多反应监测模式,并分别用APCI源和ESI源对核桃中的井冈霉素进行检测,外标法定量。结果:APCI源检测,井冈霉素在2~200 ng·mL^(-1)线性关系良好,R2=0.9983,在10μg·kg^(-1)、20μg·kg^(-1)和100μg·kg^(-1)3个浓度添加水平下,平均回收率为78.4%~98.8%,相对标准偏差为2.0%~7.8%,方法定量限为5.79μg·kg^(-1);ESI源检测,井冈霉素在2~50 ng·mL^(-1)线性关系良好,R2=0.9976,在10μg·kg^(-1)、20μg·kg^(-1)、100μg·kg^(-1)3个浓度添加水平下,平均回收率为80.7%~107.9%,相对标准偏差为1.1%~12.0%,方法定量限为8.66μg·kg^(-1)。结论:APCI源与ESI源均适用于核桃中井冈霉素的检测,灵敏度高,准确度好,重现性好。
Objective:To establish a method for the determination of Validamycin residue in walnut by ultra-high performance liquid chromatography tandem mass spectrometry.Method:Walnut samples were extracted by CH_(3)OH,purified by HLB solid phase extraction column,and separated by C_(18) column.The obtained sample was gradient eluted with a mobile phase of CH_(3)OH-0.05%ammonium acetate buffer solution.UPLC-MS/MS multi reaction monitoring mode was adopted,APCI source and ESI source were used to detect Validamycin in walnut,and external standard method was used for quantification.Result:The linearity of Validamycin was good in the concentration range of 2~200 ng·mL^(-1),R2=0.9983,at 10μg·kg^(-1),20μg·kg^(-1) and 100μg·kg^(-1).The average recovery was 78.4%~98.8%,the relative standard deviation was 2.0%~7.8%,and the limit of quantification was 5.79μg·kg^(-1);According to ESI source detection,Validamycin has a good linear relationship in the concentration range of 2~50 ng·mL^(-1),R2=0.9976,in the range of 10μg·kg^(-1),20μg·kg^(-1),100μg·kg^(-1).The average recovery was 80.7%~107.9%,the relative standard deviation was 1.1%~12.0%,and the limit of quantification was 8.66μg·kg^(-1).Conclusion:Both APCI source and ESI source are suitable for the determination of Validamycin in walnut with high sensitivity,accuracy and reproducibility.
作者
孙嵘
SUN Rong(Gratech Co.,Ltd.,Shanghai 201315,China)
出处
《现代食品》
2022年第18期197-201,共5页
Modern Food
关键词
井冈霉素
液相色谱-串联质谱
APCI源
ESI源
检测
Jinggangmycin
liquid chromatography-tandem mass spectrometry
APCI source
ESI source
detection
