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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 compare the HPLC method of Chinese Pharmacopoeia and the international standard color-value method to detect the differences of crocin in crocus sativus and to establish a more universal method for the determination of crocin in the production and distribution. Methods: The chromatographic peaks of saffron yellow at 440 nm were identified by HPLC-DAD-ESI-MS-n. Based on the results, the highest content of crocin-I was used as control, Crocin content; using this method for 62 batches of crocus samples were analyzed. Results: At 440 nm wavelength, there are four main chromatographic peaks, all crocin ingredients, the other components at this wavelength without interference, and crocin-I and II relative content highest. The determination results of 62 batches of samples showed significant linear correlation with the total content of crocin-Ⅰ and Ⅱ determined by Chinese Pharmacopoeia and the color values determined by reference to international standards. Chinese Pharmacopoeia crocetin-Ⅰ and Ⅱ total content should be above 10%, corresponding to the crocin color value of 150 or more. Conclusion: When using crocetin-Ⅰ as control, the content of crocetin-Ⅰ can be determined by UV method. The color value determined by UV method is more than 150, Samples with a price of less than 100 can be judged as unqualified products, and samples with a color value of 100-150 are respectively determined by international standards and Chinese Pharmacopoeia standards to determine whether they meet the safflower medicinal or food standards. The method provides a bridge between the Chinese Pharmacopoeia and international standards and provides a reference for the quality control widely used in the production and distribution of saffron.