摘要
目的：建立免疫亲和柱净化-高效液相色谱法测定红曲制品中桔霉素含量的分析方法。方法试样经甲醇-水提取,稀释过滤后经含桔霉素特异性抗体的免疫亲和柱净化,洗脱液经Merk Hibar RP-18e色谱柱分离,以乙腈：0.1%磷酸水溶液作为流动相,采用荧光检测器测定（激发波长350 nm,发射波长500 nm）,以外标法定量。结果桔霉素在1~50 ng/mL范围内有良好的线性关系,相关系数为0.99991,方法检测限为50μg/kg,在50、100和200μg/kg 3个水平的加标回收率为67.55%~89.12%,相对标准偏差为5.43%~11.25%。结论该方法操作简便、准确,可适用于红曲制品中桔霉素的测定。
Objective To establish a method for the determination of citrinin in monascus products by high performance liquid chromatography combined with immunoaffinity column. Methods Samples were extracted with methanol-water solution, purified by a immunoaffinity column containing specific antibody of citrinin after dilution and filteration. The eluate was separated by Merk Hibar RP-18e column with acetonitrile and 0.1%H3PO4-water as mobile phase, and detected by fluorescence detector with the excitation wavelength of 350 nm and the emission wavelength of 500 nm. Also the external standard method was used for quantitative analysis. Results Citrinin had a good linear relationship in the range of 1~50 ng/mL with correlation coefficient of 0.99991. The limit of detection was 50μg/kg. The recoveries of citrinin spiked at 3 levels of 50, 100 and 200μg/kg were 67.55%~89.12%, and the relative standard deviations were 5.43%~11.25%. Conclusion This method is simple, accurate and is suitable for the determination of citrinin in monascus products.
作者
许艳丽
吴振兴
何晓霞
静平
梁君妮
梁成珠
XU Yan-Li WU Zhen-Xing HE Xiao-Xia JING Ping LIANG Jun-Ni LIANG Cheng-Zhu(Inspection and Quarantine Center of Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266001, China QingDao Entry-Exit Inspection and Quarantine Bureau, Qingdao 266001, China Yantai Entry-Exit Inspection and Quarantine Bureau, Yantai 261400, China)
出处
《食品安全质量检测学报》
CAS
2016年第11期4649-4652,共4页
Journal of Food Safety and Quality
基金
青岛市创业创新领军人才计划(13-CX-28)~~
关键词
桔霉素
红曲制品
免疫亲和柱
高效液相色谱法
citrinin
monascus products
immunoaffinity column
high performance liquid chromatography
