西红花苷对照提取物的定值及不确定度评估研究

目的: 对西红花苷对照提取物准确赋值,并评估特性量值的不确定度。方法: 按中国药典2010 年版一部西红花项下HPLC 分析方法,以西红花苷Ⅰ和西红花苷Ⅱ为指标考察对照提取物的均匀性,5 家实验室协作定值,并评估不确定度。结果: 对照提取物的均匀性良好,西红花苷Ⅰ和西红花苷Ⅱ的标示含量和扩展不确定度分别为(68.9±1.9)% 和(23.0±0.9)%。结论: 通过协作定值及不确定度评估可实现西红花苷对照提取物的可靠赋值。

Objective: To specify the crocin reference extract and evaluate the uncertainty of the results. Methods: The uniformity of reference extract was investigated by determination of crocin Ⅰ and crocin Ⅱ using the HPLC method described in Croci Stigma that was collected in Chinese pharmacopoeia,Edition 2010.Five laboratories participated in the collaborative calibration study. The uncertainties of results were evaluated. Results: The reference extract was uniform. The marked values and extended uncertainties of the 2 components were (68.9±1.9)% and(23.0±0.9)%,respectively. Conclusion: The crocin reference extract was specified based on the results of collaborative calibration and uncertainty evaluation.

[1] 中国药典2010 年版.一部[S].2010:120 ChP 2010.Vol Ⅰ[S].2010:120
[2] 付小梅,王铮涛.西红花苷-Ⅰ的稳定性研究[J].食品科学, 2012,33(5):71 FU XM,WANG ZT.An investigation into the stability of crocin-1 [J].Food Sci,2012,33(5):71
[3] CHEN Y,CAI L,ZHAO C,et al.Spectroscopic,stability and radical-scavenging properties of a novel pigment from gardenia[J].Food Chem,2008,109(2):269
[4] VICKACKAITE V,ROMANI A,PANNACCI D,et al.Photochemical and thermal degration of a naturally occurring dye used in artistic painting.A chromatographic,spectrophotometric and fluorimetric study on saffron[J].Int J Photoenergy,2004,6(4):175
[5] TSIMIDOU M,TSATSARONI E.Stability of saffron pigment in aqueous extracts[J].J Food Sci,1993,58(5):1073
[6] 蔡仕宁,陈阳.不同结构西红花苷稳定性的研究[J].食品科技, 2012,37(8):212 CAI SN,CEHN Y.Stability investigation of different crocins[J].Food Sci Technol,2012,37(8):212
[7] 何风艳,戴忠,何轶,等.西红花苷对照提取物的研究及其在西红 花饮片质量控制中的应用[J].中国中药杂志, 2015,40(12): 2378 HE FY,DAI Z,HE Y,et al.Study on crocins reference extract and application on assay of Croci Stigma[J].China J Chin Mater Med, 2015,40(12):2378
[8] ISO Guide 35:2006 Reference Materials-General and Statistical Principles for Certification.The Third Edition[S].2006
[9] JJG 1006—1994 一级标准物质规范[S].1994 JJG 1006-1994 Technical Norm of Primary Reference Materials[S].1994
[10] JJG 1343—2012 标准物质定值的通用原则及统计学原理[S].2012 JJG 1343—2012 General and Statistical Principles for Charcaterization of Reference Materials[S].2012
[11] 姚尚辰,常艳,胡昌勤.HPLC 用β-内酰胺类抗生素化学对照 品的不确定度分析[J].药物分析杂志,2010,30(11):2104 YAO SC,CHANG Y,HU CQ.Study of uncertainty of β-lactam antibiotics chemical reference substance being used in HPLC[J].Chin J Pharm Anal,2010,30(11):2104
[12] 张卫平,蒋锦锋,王雨凝,等.三乙酸甘油酯中环己酮溶液标准物 质的研制[J].浙江工业大学学报,2013,41(3):289 ZHANG WP,JIANG JF,WANG YN,et al.Certified reference material preparation of cyclehexanone solution in triacetin[J].J Zhejiang Univ Technol,2013,41(3):289
[13] 孙茜.海洋石油污染监测苊标准物质的研制[J].海洋环境科 学,2006,35(3):93 SUN Q.Preparation of oil standard for marine monitoring[J].Mar Environ Sci,2006,35(3):93
[14] 郑小敏.高钛渣系列标准样品的研制[J].冶金分析,2012,32 (1):75 ZHENG XM.Development of certified reference materials series of high titanium slag[J].Metal Anal,2012,32(1):75
[15] 胡震,王义明,罗国安,等.栀子药材中三种有效成分HPLC 定量 分析结果不确定度的评定[J].中药材,2005,28(11):993 HU Z,WANG YM,LUO GA,et al.Estimation of measurement uncertainty of analytical results for the determination of three active component from Gardenin jasminoides Eillis.by HPLC[J].J Chin Med Mater,2005,28(11):993
[16] 胡坪,罗国安,赵中振,等.中药材定量分析中测量不确定度的评 定方法及其影响因素的研究[J].药物分析杂志,2005,25(4): 455 HU P,LUO GA,ZHAO ZZ,et al.Study on the evaluation mechod and the affecting factor of measurement uncertainty for the determination of marker compounds in Chinese materia medica[J].Chin J Pharm Anal,2005,25(4):455
[17] 胡坪,罗国安,赵中振,等.人参中人参皂苷HPLC 定量方法的测 量不确定度的评定[J].药学学报,2005,40(1):49 HU P,LUO GA,ZHAO ZZ,et al.Evaluation of measurement uncertainty for the determination of ginsenisides in Radix Ginseng by HPLC[J].Acta Pharm Sin,2005,40(1):49