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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nifdc.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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HPLC相对保留时间法中参照物的优选

Optimal selection of reference compound for HPLC relative retention time

分类号:R917
出版年·卷·期(页码):2020,40 (3):420-428
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:提出并建立相对保留时间法中参照物的优选原则,以提高该法的准确度和重现性。方法:在2台高效液相色谱仪和15根不同品牌和型号的C18色谱柱上,记录4种色谱条件下、3种中药中26个成分的保留时间,一方面对实测保留时间进行统计分析,另一方面基于推导的ΔtR(ΔtR是指保留时间实测值与保留时间计算值差的绝对值)公式进行推导分析。结果:参照物的选择对计算效果的影响较大,应选择保留时间覆盖率(保留时间覆盖率反映了参照物在整个保留时间段上的相对位置。当参照物为第一个成分时,保留时间覆盖率为0,当参照物为最后一个成分时,为100%)在50%~100%的成分为参照物,其中,60%~90%最优;选择非线性偏离较小的成分作为参照物。结论:该原则简单、准确,具有普适性,可以提高相对保留时间法的准确度和重现性。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: In order to improve the accuracy and reproducibility of the relative retention time method,the optimal selection principle of reference compound is proposed and established. Methods: The retention times of 26 compounds in 3 traditional Chinese medicines were recorded by 2 HPLC instruments using 4 kinds of chromatographic conditions and 15 ODS columns with different manufacturers and brands. Firstly,statistical analysis of the measured retention time was carried out. Secondly,based on the deduced formulas of ΔtRtR was the absolute value of the difference between the measured retention time and the calculated retention time),the deduction and analysis were performed. Results: The selection of reference compound had a great influence on the calculation results. Based on above studies,the principle for selecting reference compound for HPLC relative retention was proposed,including:(1) Selecting those compounds with 50%-100% coverage of retention time (The coverage of retention time stands for the relative position of a compound between first eluted compound and last eluted compound. For example,coverage of first compound is zero and 100% for last compound.) and the optimal coverage was 60%~90%. (2) Choosing compounds with smaller linear deviation. Conclusion: The principle is simple,accurate and universal. It can improve the accuracy and reproducibility of the relative retention time method.

-----参考文献:---------------------------------------------------------------------------------------
[1] HOU JJ,WU WY,LIANG J,et al.A single,multi-faceted,enhanced strategy to quantify the chromatographically diverse constituents in the roots of Euphorbia kansui[J].J Pharm Biomed Anal,2014,88:321
[2] WU X,HE J,XU H,et al.Quality assessment of Cinnamomi Ramulus by the simultaneous analysis of multiple active components using high-performance thin-layer chromatography and high-performance liquid chromatography[J].J Sep Sci,2014,37(18):2490
[3] LIAO H,LI Q,LIU R,et al.Fingerprint analysis and multi-ingredient determination using a single reference standard for Saposhnikoviae radix[J].Anal Sci,2014,30(12):1157
[4] DA J,CHENG CR,YAO S,et al.A reproducible analytical system based on the multi-component analysis of triterpene acids in Ganoderma lucidum[J].Phytochemistry,2015,114:146
[5] DÓRA V,YVAN V H,TÍMEA I,et al.Characterisation of reversed-phase liquid chromatographic columns by chromatographic tests.Evaluation of 36 test parameters:repeatability,reproducibility and correlation[J].J Chromatogr A,2002,977(1):39
[6] WILSON NS,NELSON MD,DOLAN JW,et al.Column selectivity in reversed-phase liquid chromatography I.A general quantitative relationship[J].J Chromatogr A,2002,961(2):171,195,217
[7] WHELAN TJ,GRAY MJ,SLONECKER PJ,et al.Study of the selectivity of reversed-phase columns for the separation of polycarboxylic acids and polyphenol compounds[J].J Chromatogr A,2005,1097(1-2):148
[8] BACZEK T,KALISZAN R,NOVOTNA K,et al.Comparative characteristics of HPLC columns based on quantitative structure-retention relationships (QSRR) and hydrophobic-subtraction model[J].J Chromatogr A,2005,1075(1-2):109
[9] SNYDER LR,DOLAN JW,CAR PW.A new look at the selectivity of RPC columns.The hydrophobic subtraction model evaluates the selectivity of HPLC reversed-phased columns so that researchers can choose a suitable substitute or a sufficiently orthogonal second column[J].Anal Chem,2007,79(9):3254
[10] GILROY J J,DOLAN J W,SNYDEER L R.Column selectivity in reversed-phase liquid chromatography:IV.Type-B alkyl-silica columns[J].J Chromatogr A,2003,1000(1-2):757
[11] GILROY J J,DOLAN J W,CARR P W,et al.Column selectivity in reversed-phase liquid chromatography:V.Higher metal content (type-A) alkyl-silica columns[J].J Chromatogr A,2004,1026(1-2):77
[12] WILSON NS,GILORY J,DOLAN JW,et al.Column selectivity in reversed-phase liquid chromatography:VI.Columns with embedded or end-capping polar groups[J].J Chromatogr A,2004,1026(1-2):91
[13] VISKY D,HEYDEN YV,IVANYI T,et al.Characterisation of reversed-phase liquid chromatographic columns by chromatographic tests:Rational column classification by a minimal number of column test parameters[J].J Chromatogr A,2004,1012(1):11
[14] DEHOUCK P,VISKY D,HEYDEN YV,et al.Characterisation of reversed-phase liquid-chromatographic columns by chromatographic tests:comparing column classification based on chromatographic parameters and column performance for the separation of acetylsalicylic acid and related compounds[J].J Chromatogr A,2004,1025(2):189
[15] VISKY D,HAGHEDOOREN E,DEHOUCK P,et al.Facilitated column selection in pharmaceutical analyses using a simple column classification system[J].J Chromatogr A,2006,1101(1-2):103
[16] KOCZIAN K,HAGHEDOOREN E,DRAGOVIC S,et al.Column selection for pharmaceutical analyses based on a column classification using four test parameters[J].J Pharm Biomed Anal,2007,44(4):894
[17] SNYDER LR,DOLAN JW,CARR PW.The hydrophobic-subtraction model of reversed-phase column selectivity[J].J Chromatogr A,2004,1060(1-2):77
[18] DOLAN JW,MAULE A,BINGLEY D,et al.Choosing an equivalent replacement column for a reversed-phase liquid chromatographic assay procedure[J].J Chromatogr A,2004,1057(1-2):59
[19] DRAGOVIC S,HAGHEDOOREN E,NEMETH T,et al.Evaluation of two approaches to characterise liquid chromatographic columns using pharmaceutical separations[J].J Chromatogr A,2009,1216(15):3210
[20] 中华人民共和国药典2015年版.一部[S].2015:22 ChP 2015.VolⅠ[S].2015:22
[21] 逄瑜,孙磊,金红宇,等.指纹图谱结合化学计量学分析用于多种大黄的鉴别及质量评价[J].中国药学杂志,2014,49(4):287 PANG Y,SUN L,JIN HY,et al.Identification and quality evaluation of Radix et Rhizoma Rhei by HPLC fingerprint and chemometrics analysis[J].Chin Pharm J,2014,49(4):287
[22] 中华人民共和国香港特别行政区中药材标准.第三册[S].2012:101 Department of Health Hong Kong Special Administrative Region,the People's Republic of China,Hong Kong Chinese Material Medical Standards.Vol 3[S].2012:101
[23] 孙磊,张超,田润涛,等.色谱指纹图谱结合化学计量学用于3种乳香的鉴别和质量评价[J].中国药学杂志,2015,50(2):140 SUN L,ZHANG C,TIAN RT,et al.A Holistic strategy of identification and quality evaluation of frankincense by chromatographic fingerprint combined with chemometrics[J].Chin Pharm J,2015,50(2):140
[24] 王龙星,肖红斌,梁鑫淼.一种提高色谱指纹谱保留时间重现性的新方法[J].分析化学,2003,31(10):1232 WANG LX,XIAO HB,LIANG XM.A new method to improve the reproducibility of retention time on reversed phase C18 columns in different laboratories[J].Chin J Anal Chem,2003,31(10):1232
[25] SUN L,JIN H,TIAN R,et al.A simple method for HPLC retention time prediction:linear calibration using two reference substances[J].Chin Med,2017,12(1):16

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