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采用固相萃取与液相色谱-串联质谱联用技术分离和定量测定羌活根茎中的羌活醇对映异构体。

Separation and quantitation of notopterol enantiomers in notopterygii rhizoma et radix using solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry.

机构信息

School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenhe District, Shenyang, 110016, PR China.

School of Pharmacy, Shenyang Pharmaceutical University, No. 103 Wenhua Road, Shenhe District, Shenyang, 110016, PR China.

出版信息

J Pharm Biomed Anal. 2020 Jul 15;186:113255. doi: 10.1016/j.jpba.2020.113255. Epub 2020 Mar 23.

Abstract

In this study, a specific, sensitive, and reliable high performance liquid chromatography-tandem mass spectrometry method has been developed and validated for the quantitative determination of notopterol enantiomers in Notopterygii Rhizoma et Radix. Solid-phase extraction was used for the extraction of notopterol enantiomers from Notopterygii Rhizoma et Radix. Enantiomeric separation of notopterol was achieved on a Chiralpak IA column with the mobile phase consisting of acetonitrile-water (50:50, v/v) at a flow rate of 0.6 mL/min. Quantification was performed on a triple quadrupole tandem mass spectrometry equipped with an electrospray ionization source in the positive ionization and multiple reaction monitoring mode. The lower limit of quantification and lower limit of detection were 0.09 and 0.04 mg/g for each enantiomer in NRR samples. And each enantiomer showed good linearity (R≥0.999) in the range of 0.09-9.55 mg/g. The precision, repeatability, and stability were all within satisfaction. The average recoveries of (-)-notopterol and (+)-notopterol were demonstrated to be 99.3 % and 101.1 %, respectively, with the relative standard deviations less than 5.0 %. Finally, the validated method was successfully applied to the quantification of notopterol enantiomers in Notopterygii Rhizoma et Radix from different sources.

摘要

本研究建立并验证了一种专属性强、灵敏度高、重现性好的高效液相色谱-串联质谱法,用于定量测定独活药材中羌活醇对映体的含量。采用固相萃取法从独活药材中提取羌活醇对映体,以乙腈-水(50:50,v/v)为流动相,在 Chiralpak IA 柱上进行对映体分离,流速为 0.6 mL/min。采用电喷雾正离子源和三重四极杆串联质谱,在多反应监测模式下进行定量分析。该方法的定量下限和检测下限分别为 0.09 和 0.04 mg/g。羌活醇对映体在 0.09-9.55 mg/g 范围内均具有良好的线性关系(R≥0.999)。精密度、重复性和稳定性均符合要求。(-)-羌活醇和(+)-羌活醇的平均回收率分别为 99.3%和 101.1%,相对标准偏差均小于 5.0%。最后,该方法成功应用于不同来源独活药材中羌活醇对映体的含量测定。

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