标准研讨

UPLC-MS/MS法同时测定药用及观赏芍药中15个成分*

展开
  • 1.兰州市食品药品检验检测研究院/甘肃省种植中药材外源性污染物监测工程研究中心,兰州 730050;
    2.国家市场监管重点实验室(食品中农药兽药残留监控),兰州 730050;
    3.兰州市农业科技研究推广中心,兰州 730050
第一作者 Tel:(0931)2317718;E-mail:58748741@qq.com

收稿日期: 2021-02-24

  网络出版日期: 2024-06-26

基金资助

*甘肃省重点研发项目(18YF1NA138);甘肃省市场监督管理局科技计划项目(SSCJG-SP-201910、SSCJG-SP-202121)

Simultaneous determination of 15 components in medicinal and ornamental peony by UPLC-MS/MS*

Expand
  • 1. Lanzhou Institute for Food and Drug Inspection and Testing, Lanzhou 730050, China;
    2. Gansu Engineering Research Center for Monitoring Exogenous Harmful Residues in Traditional Chinese Medicines, Lanzhou 730050, China;
    3. Lanzhou Agricultural Science and Technology Research and Extension Center, Lanzhou 730050, China

Received date: 2021-02-24

  Online published: 2024-06-26

摘要

目的: 建立超高效液相色谱-三重四极杆质谱法(UPLC-MS/MS)同时测定芍药中15个成分含量。方法: 采用Waters UPLC HSS T3 (150 mm×2.1 mm,1.8 μm)色谱柱,以乙腈(A)-5 mmol·L-1乙酸铵+0.1%甲酸水溶液(B)为流动相,梯度洗脱(0~1.0 min,10%A→15%A;1.0~6.0 min,15%A→30%A;6.0~10.0 min,30%A→90%A;10.0~12.0 min,90%A→10%A),流速0.30 mL·min-1,电喷雾离子源(ESI),正、负离子模式下扫描,采用多重反应监测模式(MRM)。结果: 15个成分在考察的浓度范围内呈良好的线性关系(r>0. 995),检测下限范围为0.039 08~25.45 mg·kg-1, 定量下限范围为0.130 3~84.83 mg·kg-1,回收率为90.6%~96.0%,RSD为2.7%~5.4%。结论: 所建立方法操作简便,分析速度快,灵敏度高,重复性、回收率良好,可用于芍药中多个成分的含量测定。

本文引用格式

张文, 朱仁愿, 李洁, 闫君, 赵亚兰, 王行智, 代立兰 . 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 -493 . DOI: 10.16155/j.0254-1793.2022.03.16

Abstract

Objective: To establish a method for simultaneous determination of 15 components in Paeonia lactiflora by ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). Methods: Determination was carried out on a Waters UPLC HSS T3 column (150 mm×2.1 mm, 1.8 μm). The mobile phase was composed of 0.1% formic acid containing 5 mmol·L-1 ammonium acetate (B) and acetonitrile (A) with gradient elution (0-1.0 min, 10%A→15% A;1.0-6.0 min,15%A→30%A; 6.0-10.0 min, 30%A→90%A; 10.0-12.0 min, 90%A→10%A) at a flow rate of 0.3 mL·min-1. The electrospray ionization(ESI)source was performed in multiple reaction monitoring (MRM) mode using positive and negative electrospray ionization. Results: Under the optimized chromatographic conditions, good separation of 15 target components was obtained within 12 min. Satisfactory linearity was achieved within the investigated linear ranges and with fine coefficients (r>0.995). The detection limits were 0.039 08-25.45 mg·kg-1, the limits of quantification were 0.130 3-84.83 mg·kg-1, the recoveries were 90.6%-96.0%, and the RSDs were 2.7%-5.4%. Conclusion: It is the first report of simultaneous analysis of 15 kinds of components in peony’s root by using UPLC-MS/MS method. The method is simple, fast, sensitive, reproducible and of good recovery, which can be used for the determination of components in Paeonia lactiflora.

参考文献

[1] 中华人民共和国药典 2020 年版.一部[S].2015:108,165
ChP. Vol Ⅰ[S].2015:108,165
[2] 康晓飞,郭先锋,许世磊,等.三个观赏芍药品种芍药苷含量的动态变化研究[J].北方园艺,2011(5):85
KANG XF, GUO XF, XU SL, et al. Study on dynamic changes of paeoniflorin content in three ornamental varieties of Paeonia lactiflora[J].Northern Hortic,2011(5):85
[3] 周晓君,张凯,彭正锋,等.矮牡丹与芍药属其他5个种叶绿体基因组特征的比较[J].林业科学,2020,56(4):82
ZHOU XJ, ZHANG K, PENG ZF, et al. Comparative Analysis of Chloroplast Genome Characteristics between Paeonia jishanensis and other five species of paeonia[J].Scientia Silvae Sinicae, 2020, 56(4):82
[4] 何泽源,张妍妍,林楠,等. 赤芍化学成分和药理作用及质量标志物的预测分析[J].中药材,2020,43(12):3075
HE ZY, ZHANG YY, LIN N, et al. Predictive analysis of chemical constituents, pharmacological effects and quality markers of Paeoniae Radix Rubra[J].Chin Mater Med, 2020, 43(12):3075
[5] 叶先文, 夏澜婷, 任洪民, 等.白芍炮制的历史沿革及化学成分、药理作用研究进展[J].中草药, 2020, 51(7):1951
YE XW, XIA LT, REN HM, et al. Research progress on processing history evolution, chemical constituents and pharmacological action of Paeoniae Radix Alba[J].Chin Traditional and Herbal Drugs, 2020, 51(7):1951
[6] PARKER S, MAY B, ZHANG C, et al. A Pharmacological review of bioactive constituents of Paeonia lactiflora Pallas and Paeonia veitchii Lynch[J].Phytother Res, 2016, 30:1445
[7] 亓超, 郑重飞, 李莹, 等.川赤芍的化学成分分离鉴定[J].中国实验方剂学杂志, 2020, 26(6):152
QI C, ZHEN ZF, LI Y, et al. Isolation and identification of chemical constituents from Paeonia veitchii[J].Chin J Exp Tradit Med Form, 2020, 26(6):152
[8] 梁文娟, 尹迪, 郗建宇, 等.美丽芍药根中黄酮类成分及其生物活性[J].中成药, 2021, 43(2):399-403.
LIANG WJ, YI D, XI JY, et al. Flavonoids from the roots of Paeonia mairei and their biological activities[J].Chin Tradit Pat Med, 2021, 43(2):399
[9] 石钰, 马养民, 康永祥, 等.美丽芍药化学成分[J].中国实验方剂学杂志, 2014, 20(23):104
SHI Y, MA YM,KANG YX, et al. Chemical Compositions of Paeonia mairei[J].Chinese Journal of Experimental Traditional Medical Formulae, 2014, 20(23):104
[10] YANG Y, LI SS, JAIME A. TEIXEIRA DA SILVa, et al. Characterization of phytochemicals in the roots of wild herbaceous peonies from China and screening for medicinal resources[J].Phytochemistry, 2020,174:1
[11] 冯一涵, 殷蕾, 刘远荣, 等.杭白芍九种主要成分的高效液相色谱定量分析及提取工艺研究[J].浙江大学学报(医学版), 2020, 49(3):356
FEN YH, YIN L, LIU YR, et al. Quantitative determination and optimun extraction technique of nine compounds of Paeoniae Radix Alba[J].J Zhejiang Univ(Med Sci), 2020, 49(3):356
[12] 于现花, 高海燕, 金传山, 等. 不同产地白芍标准煎液的指纹图谱及4种单萜苷类成分含量测定[J].中国现代应用药学, 2020, 37(11):1290
YU XH, GAO HY, JIN CS, et al. Fingerprint of Paeoniae Radix Alba standard decoction from different producing areas and determination of four monoterpenoid glycosides components[J].Chin J Mod Appl Pharm, 2020, 37(11):1290
[13] 刘杰, 陈琳, 范彩荣, 等. 基于HPLC-DAD-Q-TOF-MS/MS的白芍和赤芍主要成分定性定量研究[J].中国中药杂志, 2015, 40(9):1762
LIU J, CHEN L, FAN CR, et al. Qualitative and quantitative analysis of major constituents of Paeoniae Radix Alba and Paeoniae Radix Rubra by HPLC-DAD-Q-TOF-MS/MS[J].Chin J Chin Mater Med, 2015, 40(9):1762
[14] HE CN, PENG B, DAN Y, et al. Chemical taxonomy of tree peony species from China based on root cortex metabolic fingerprinting[J].Phytochemistry, 2014, 107:69.
[15] 刘杰, 许文, 李煌, 等. UPLC-MS/MS法同时测定白芍饮片中10种成分[J].药物分析杂志, 2015, 35(4):635
LIU J, XU W, LI H, et al. Simultaneous determination of ten components in Radix Paeoniae Alba pieces by UPLC-MS/MS[J].Chin J Pharm Anal, 2015, 35(4):635
[16] 任浚萁, 刘春明, 王乐奇, 等. 白芍化学成分的高效液相色谱-电喷雾质谱研究[J].药物分析杂志, 2014, 34(10):1727
REN JQ, LIU CM, WANG LQ, et al. Determination of chemical compositions in extract of Radix Paeoniae Alba by liquid chromatography-electrospray ionization mass spectrometry[J].Chin J Pharm Anal, 2014, 34(10):1727
[17] 苏红, 何峰, 刘志宝, 等. UPLC-MS-MS法同时检测大鼠血浆中没食子酸和芍药苷的浓度及其药代动力学研究[J].中国实验方剂学杂志, 2014, 20(4):94
SU H, HE F, LIU ZB, et al. Simultaneous determination and pharmacokinetics of gallic acid and paeoniflorin in rat plasma by UPLC-MS-MS[J].Chin J Exp Tradit Med Form, 2014, 20(4):94-98
[18] YANG GD, ZHANG CH, LI P, et al. Chemical fingerprinting and quantitative analysis of cortex moutan from different tree peony cultivars using HPLC-ESI/MS[J].Nat Product Commun, 2020, 15(11):1
[19] 李凤玉,曹阳,韩行舟. 牡丹江地区芍药根中主要活性成分的研究与探讨[J].中国林副特产,2020,35(1):9
LI FY, CAO Y, HAN XZ. Research and Discussion on the Main Active Components in Paeonia lactiflora Roots in Mudanjiang[J].Forest Pro Spec China, 2020, 35(1):9
文章导航

/