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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/m L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 an analytical method for the determination of citrinin in Monascus preparations by immunoaffinity column cleanup and high performance liquid chromatography. Methods The samples were extracted with methanol-water, diluted by filtration and purified by immunoaffinity column with citrinin-specific antibody. The eluate was separated on a Merk Hibar RP-18e column using acetonitrile: 0.1% phosphoric acid as mobile phase , Using a fluorescence detector (excitation wavelength 350 nm, emission wavelength 500 nm), external standard method. Results The calibration curve of citrinin was linear in the range of 1 ng / mL to 50 ng / mL with a correlation coefficient of 0.99991. The limit of detection was 50 μg / kg. The spiked recoveries at three levels of 50, 100 and 200 μg / kg were 67.55% ~ 89.12%, the relative standard deviation was 5.43% ~ 11.25%. Conclusion The method is simple and accurate and can be applied to the determination of citrinin in Monascus preparations.