基于中国药典与国际标准对西红花生产流通中质量评价方法的改良

Improvement of quality evaluation of Croci Stigma in the process of producing and distributing based on Chinese pharmacopoeia and ISO

目的:比较中国药典的HPLC法和国际标准的色价法检测西红花中西红花苷的差异,建立更能普遍适用于生产流通中检测总西红花苷含量的方法。方法:采用HPLC-DAD-ESI-MS^n对西红花440 nm波长下的色谱峰进行结构鉴定,在此基础上,以含量最高的西红花苷-Ⅰ为对照,建立UV法测定总西红花苷的含量;采用该方法对62批西红花样品进行分析。结果:440 nm波长下主要有4个色谱峰,均为西红花苷类成分,其他类成分在此波长无干扰,并且西红花苷-Ⅰ和Ⅱ相对含量最高。62批样品的测定结果与按中国药典测定的西红花苷-Ⅰ、Ⅱ总含量及参考国际标准测定的色价均有显著线性相关性。中国药典规定西红花苷-Ⅰ和Ⅱ总含量应在10%以上,相应西红花苷色价均在150以上。结论:对总西红花苷定量时,可以西红花苷-Ⅰ为对照,用UV法对其含量进行测定;并将UV法测定的色价大于150作为快速判定药材合格的标准,对色价小于100的样品可判为不合格品,色价为100～150间的样品需分别用国际标准与中国药典标准进行测定,以判别是否符合西红花药用标准或食品标准。该方法在中国药典与国际标准间架起了一个桥梁,为普遍用于西红花生产流通中的质量监控提供了参考。

Objective：To explore an efficient,convenient and feasible method for the contents determination of total crocins in Croci Stigma based on Chinese pharmacopoeia（Ch P） — HPLC method and ISO — color value.Methods：Firstly,ESI-MS^n was adopted to identify the peaks at the wavelength of 440 nm,and crocin-Ⅰ was used as the reference for UV method of content determination of total crocins from 62 batches of Croci Stigma.Results：The results showed all the peaks were crocins,without other peaks,and the contents of crocins-Ⅰ and crocins-Ⅱ were the highest.There was a significant linear correlation between the contents of total crocins determined by UV,total contents of crocins-Ⅰ and crocins-Ⅱ determined by Ch P-HPLC and the improved color value determined by ISO.Ch P requires that total contents of crocins— and crocins-Ⅱ should be more than 10%,correspondingly the color value should be more than 150.Conclusion：UV can be adopted for the content determination of total crocins,and crocin-Ⅰ can be used as the reference.In addition,when determining whether Croci Stigma is qualified,the color value above 150 can be used as the fast determination standard.When the color value is less than 100,the sample can be identified as unqualified.When the color value is in the range of 100-150,the sample should be identified by Ch P—HPLC and ISO—color value to identify whether it meets the medicinal standards or international food standards.The presented method has been a bridge between Ch P and ISO,and provides a reference for quality control of Croci Stigma in the process of producing and distributing.