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目的:建立血脂康胶囊中桔霉素的HPLC检测方法,并同时考察数批市售相关红曲产品中桔霉素的含量。方法:采用HPLC法,色谱柱:Aichrombond-AQ C_(18)柱(250mm×4.6mm,5μm),流动相:乙腈-水(磷酸调节pH 2.5),梯度洗脱,柱温:28℃,流速:1.0ml·min~(-1),荧光检测,波长:λ_(ex)=331nm、λ_(ex)=500 nm。结果:桔霉素在0.21~10.74ng范围内线性关系良好(r=0.999 9),最低检测限为0.003 7ng。血脂康胶囊及红曲保健品中均未检出桔霉素,而其他红曲产品中检出桔霉素,其含量在0.1~549.0mg·kg~(-1)范围内不等。结论:方法准确、灵敏度高,可有效地控制血脂康胶囊及其他红曲产品质量。
Objective: To establish an HPLC method for the determination of citrinin in Xuezhikang Capsules. At the same time, the content of citrinin in several batches of commercially available Monascus products was also investigated. Methods: Aichrombond-AQ C_ (18) column (250 mm × 4.6 mm, 5 μm) was used as the mobile phase. The mobile phase consisted of acetonitrile and water (adjusted to pH 2.5 with phosphoric acid) : 1.0ml · min -1, Fluorescence detection, λ = (ex) = 331nm, λex (ex) = 500nm. Results: The linear range of citrinin was 0.21 ~ 10.74ng (r = 0.999 9), the lowest detection limit was 0.003 7ng. No samples of citrinin were found in Xuezhikang and Hongqu health products, while citrinin was detected in other products of Hongqu, the contents ranged from 0.1 to 549.0 mg · kg ~ (-1). Conclusion: The method is accurate and sensitive, which can effectively control the quality of Xuezhikang capsules and other red yeast rice products.