成分分析

HPLC-MS/MS法同时测定心脑静片中10个成分的含量*

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  • 1.中国食品药品检定研究院,北京 100050;
    2.中国中医科学院医学实验中心,北京 100700
第一作者 Tel:(010)67095424;E-mail:hfy_198616@163.com
**张海鸣 Tel:(010)64089536;E-mail:157843684@qq.com
马双成 Tel:(010)53852076;E-mail:masc@nifdc.org.cn

修回日期: 2023-02-27

  网络出版日期: 2024-06-25

基金资助

*国家药品标准制修订研究课题(2021Z15)

Simultaneous determination of 10 components in Xinnaojing tablets by HPLC-MS/MS*

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  • 1. National Institutes for Food and Drug Control, Beijing 100050, China;
    2. Experimental Research Center, China Academy of Chinese Medical Sciences, Beijing 100700, China

Revised date: 2023-02-27

  Online published: 2024-06-25

摘要

目的: 建立HPLC-MS/MS同时测定心脑静片中10个成分含量的方法。方法: 采用Agilent Zorbax Eclipse Plus C18(50 mm×2.1 mm,1.8 μm)色谱柱,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,流速为0.4 mL·min-1,柱温为30 ℃,进样量为1 μL;质谱采用负离子扫描,多反应监测(MRM)模式进行定量分析。结果: 10个成分在一定浓度范围内与峰面积呈良好线性关系,线性相关系数r均>0.999 0;平均回收率(n=6)在94.9%~107.9%,RSD在0.9%~3.4%。2个厂家14批样品中绿原酸、龙胆苦苷、甘草苷、甘草酸、芦丁、迷迭香酸、汉黄芩苷、黄芩素、汉黄芩素、喜果苷的含量分别为0.49~1.24、1.75~4.14、0.06~0.13、0.19~0.48、24.53~35.55、0.56~1.17、6.31~10.22、0.96~2.89、0.48~1.28、0.03~0.08 mg·g-1。除喜果苷外,不同厂家样品中其他9个成分的测定结果较为接近。结论: 本方法灵敏、准确,可用于心脑静片的质量控制。

本文引用格式

何风艳, 周亚楠, 戴忠, 张海鸣, 马双成 . HPLC-MS/MS法同时测定心脑静片中10个成分的含量*[J]. 药物分析杂志, 2023 , 43(4) : 564 -572 . DOI: 10.16155/j.0254-1793.2023.04.04

Abstract

Objective: To establish an HPLC-MS/MS method for simultaneous determination of 10 components in Xinnaojing tablets. Methods: HPLC assay was performed on Agilent Zorbax Eclipse Plus C18(50 mm×2.1 mm, 1.8 μm)column with a mixture of acetonitrile and 0.1% formic acid as the mobile phase in gradient elution at a flow rate of 0.4 mL·min-1. The column temperature was 30 ℃ and the injection volume was 1 μL. Detection was carried out on a triple quadrupole mass spectrometer in negative ion mode using an electrospray source. Multiple reaction monitoring(MRM) mode was employed. Results: All 10 components showed good linearity (r>0.999 0). The average recoveries (n=6) were in the range of 94.9%-107.9% with RSDs within 0.9%-3.4%. The contents of chlorogenic acid, gentiopicrin, liquiritin, glycyrrhizic acid, rutoside, rosmarinic acid, wogonoside, baicalein, wogonin and vincosamide in 14 tested samples from 2 manufacturers were 0.49-1.24, 1.75-4.14, 0.06-0.13, 0.19-0.48, 24.53-35.55, 0.56-1.17, 6.31-10.22, 0.96-2.89, 0.48-1.28, and 0.03-0.08 mg·g-1. Except for vincosamide, the contents of other 9 investigated components in tested samples from different manufacturers were close. Conclusion: The developed method is accurate and sensitive. It can be used in quality control of Xinnaojing tablets.

参考文献

[1] 中华人民共和国药典 2020年版. 一部[S].2020: 767
ChP 2020. VolⅠ[S].2020: 767
[2] 张多, 王明园. HPLC法同时测定心脑静片中木香内酯与去氧木香内酯的含量[J].黑龙江科技信息, 2015(15): 84
ZHANG D, WANG MY. Simultaneous determination of costunolide and dehydrocostuslactone in Xinnaojing tablets by HPLC[J].Heilongjiang Sci Technol Inf, 2015(15): 84
[3] 董晓蕾, 张霁, 赵艳丽, 等. 龙胆炮制前后化学成分变化的比较研究[J].药物分析杂志, 2015, 35(4): 620
DONG XL, ZHANG J, ZHAO YL, et al. A comparative study on chemical components of Longdan before and after processing[J].Chin J Pharm Anal, 2015, 35(4): 620
[4] 李翟, 姜大成, 翁丽丽, 等. 一测多评法同时测定龙胆不同部位中3个环烯醚萜苷类成分的含量[J].药物分析杂志, 2019, 39(6): 1069
LI D, JIANG DC, WENG LL, et al. Simultaneous determination of three iridoid glycosides in different parts of Gentianae by QAMS[J].Chin J Pharm Anal, 2019, 39(6): 1069
[5] 陈佳, 张权, 杨蕊, 等. 不同生长年限甘草主要成分含量测定及多元统计分析[J].药物分析杂志, 2020, 40(7): 1185
CHEN J, ZHANG Q, YANG R, et al. Determination and multivariate statistical analysis of chemical components in Glycyrrhizae Radix et Rhizoma with different growth years[J].Chin J Pharm Anal, 2020, 40(7): 1185
[6] 曾路, 楼之岑, 张如意. 国产甘草的质量评价[J].药学学报, 1991, 26(10): 788
ZENG L, LOU ZC, ZHANG RY. Quality evaluation of Chinese licorice[J].Acta Pharm Sin, 1991, 26(10): 788
[7] 王祝举, 赵玉英, 王邠, 等. 夏枯草中迷迭香酸含量分析方法研究[J].药物分析杂志, 2006, 26(3): 399
WANG ZJ, ZHAO YY, WANG B, et al. Studies on analytical method of rosmarinic acid in Spica Prunellae[J].Chin J Pharm Anal, 2006, 26(3): 399
[8] 方罗, 林能明, 吴永江. 高效液相色谱同时测定夏枯草药材中4种活性成分的含量[J].中国中药杂志, 2010, 35(5): 616
FANG L, LIN NM, WU YJ. Simultaneous determination of four active components in Spica Prunellae by HPLC[J].China J Chin Mater Med, 2010, 35(5): 616
[9] 辛文波, 侴桂新, 王峥涛. 钩藤生物碱类成分研究[J].中草药, 2009, 40(2): 204
XIN WB, CHOU GX, WANG ZT. Alkaloids from Uncaria rhynchophylla[J].Chin Tradit Herb Drugs, 2009, 40(2): 204
[10] XIE S, SHI Y, WANG Y, et al. Systematic identification and quantification of tetracyclic monoterpenoidoxindole alkaloids in Uncaria rhynchophylla and their fragmentations in Q-TOF-MS spectra[J].J Pharm Biomed Anal, 2013, 80-82: 56
[11] 刘金亮, 李隆云, 何光华, 等. HPLC 指纹图谱结合化学计量学与抗氧化能力评价不同产地槐米的品质[J].中草药, 2018, 49(19): 4644
LIU JL, LI LY, HE GH, et al. Quality evaluation of Flos Sophorae Immaturus from different habitats by HPLC coupled with chemometrics and anti-oxidant ability[J].Chin Tradit Herb Drugs, 2018, 49(19): 4644
[12] 韩乐, 陈巧霞, 刘训红, 等. MEKC-DAD同时测定黄芩中6个黄酮类成分的含量[J].药物分析杂志, 2013, 33(9): 1525
HAN L, CHEN QX, LIU XH, et al. Simultaneous determination of six lavonoids in Scutellariae Radix by MEKC-DAD[J].Chin J Pharm Anal, 2013, 33(9): 1525
[13] 张雪梅, 张刘伟, 何凯乐, 等. 基于HPLC指纹图谱和多指标定量的黄芩趁鲜加工研究[J].中草药, 2021, 52(15): 4552
ZHANG XM, ZHANG LW, HE KL, et al. Study on fresh processing of Scutellaria baicalensis based on HPLC fingerprint and multi-index quantification[J].Chin Tradit Herb Drugs, 2021, 52(15): 4552
[14] 何巧玉, 刘静, 李春霞, 等. 基于网络药理学和指纹图谱的黄柏质量标志物预测分析[J].中草药, 2021, 52(16): 4931
HE QY, LIU J, LI CX, et al. Predictive analysis of Phellodendri Chinensis Cortex quality markers based on network pharmacology and fingerprint[J].Chin Tradit Herb Drugs, 2021, 52(16): 4931
[15] 吴琦, 张凡, 鞠成国, 等. 黄柏及其不同炮制品的指纹图谱研究[J].亚太传统医药, 2017, 13(20): 31
WU Q, ZHANG F, JU CG, et al. Fingerprint analysis among different processed products of Phellodendri Chinensis Cortex[J].Asia Pac Tradit Med, 2017, 13(20): 31
[16] 李超, 赵权, 田刚, 等. LC-MS/MS法同时测定小儿豉翘清热颗粒中13个成分的含量[J].药物分析杂志, 2022, 42(4): 572
LI C, ZHAO Q, TIAN G, et al. Simultaneous determination of 13 components in Xiao’er Chiqiao Qingre granules by LC-MS/MS[J].Chin J Pharm Anal, 2022, 42(4): 572
[17] 袁强华, 谢凡, 谈静, 等. 银翘藿朴退热合剂中13个活性成分的定量分析[J].药物分析杂志, 2022, 42(4): 598
YUAN QH, XIE F, TAN J, et al. Quantitative analysis of 13 pharmacodynamic components in Yinqiao Huopu Tuire mixture[J].Chin J Pharm Anal, 2022, 42(4): 598
[18] 张文, 朱仁愿, 李洁, 等. UPLC-MS/MS法同时测定药用及观赏芍药中15个成分[J].药物分析杂志, 2022, 42(3): 484
ZHANG W, ZHU RY, LI J, et al. Simultaneous determination of 15 components in medicinal and ornamental peony by UPLC-MS/MS[J].Chin J Pharm Anal, 2022, 42(3): 484
[19] 温秀萍, 翁艳鸿, 陈祖倩, 等. UPLC-MS/MS法同时测定绞股蓝中16个皂苷类成分的含量[J].药物分析杂志, 2022, 42(2): 198
WEN XP, WENG YH, CHEN ZQ, et al. Determination of 16 saponins in Gynostemmatis Pentaphylli Herba based on UPLC-MS/MS[J].Chin J Pharm Anal, 2022, 42(2): 198
[20] 朱广伟, 李西文, 李琦, 等. 基于传统煎药工艺的龙胆饮片标准汤剂制备及质量评价方法研究[J].中草药, 2017, 48(20): 4253
ZHU GW, LI XW, LI Q, et al. Study on preparation and quality evaluation of standard decoction of Gentianae Radix based on traditional decocting process[J].Chin Tradit Herb Drugs, 2017, 48(20): 4253
[21] 王迎春, 王晓亚, 麻景梅, 等. 夏枯草饮片及标准汤剂质量评价相关性研究[J].中国中医药信息杂志, 2018, 25(10): 79
WANG YC, WANG XY, MA JM, et al. Correlation study on quality evaluation of decoction pieces and standard decoction of Prunellae Spica[J].Chin J Inf Tradit Chin Med, 2018, 25(10): 79
[22] 林伟雄, 乐志勇, 车海燕, 等. 甘草饮片标准汤剂的研究[J].中国中药杂志, 2017, 42(5): 830
LIN WX, LE ZY, CHE HY, et al. Research on Glycyrrhizeae Radix standard decoction[J].China J Chin Mater Med, 2017, 42(5): 830
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