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采用最佳微波萃取结合正负离子转换多反应监测(+/-MRM)技术快速测定马齿苋中八种生物活性生物碱。

Rapid determination of eight bioactive alkaloids in Portulaca oleracea L. by the optimal microwave extraction combined with positive-negative conversion multiple reaction monitor (+/-MRM) technology.

机构信息

Key Laboratory of Structure-Based Drug Design & Discovery, Ministry of Education, Shenyang Pharmaceutical University, Shenyang 110016, China; School of Traditional Chinese Materia Medica, Shenyang Pharmaceutical University, Shenyang 110016, China.

Liaoning Chengda Biotechnology Co., Ltd., Shenyang 110179, China.

出版信息

Talanta. 2014 Mar;120:167-72. doi: 10.1016/j.talanta.2013.11.067. Epub 2013 Dec 3.

Abstract

A rapid and reliable microwave extraction and the triple quadrupole-linear ion trap mass spectrometry method was developed and validated for the determination of eight alkaloids in Portulaca oleracea L. The optimal microwave extraction (MWE) condition was performed at 60 °C for 12 min with ethanol-water (70:30, v/v) as the extracting solvent, and the solvent to solid ratio was 30:1. The alkaloids were first detected simultaneously by electrospray ionization tandem mass spectrometry under positive-negative conversion multiple reaction monitor ((+/-)MRM) technique. With investigating three different columns, samples were separated in only 8 min on a Waters ACQUITY UPLC HSS T3 (50 × 2.1 mm(2), 1.8 μm) column using acetonitrile and formic acid-water solution as a mobile phase with a flow rate at 0.2 mL/min. All calibration curves showed good linearity (r>0.999) within the test ranges. The method developed was validated with acceptable sensitivity, intra- and inter-day precision, reproducibility, and extraction recoveries. It was successfully applied to the determination of eight alkaloids in Portulaca oleracea L. from different sources and different harvest periods. The method also provide a reference for extraction and determination of alkaloids in other complex systems.

摘要

建立并验证了一种快速、可靠的微波萃取三重四极杆-线性离子阱质谱法,用于测定马齿苋中 8 种生物碱。最佳微波萃取(MWE)条件为 60°C 下用乙醇-水(70:30,v/v)作为提取溶剂萃取 12min,溶剂与固体的比例为 30:1。采用电喷雾电离串联质谱在正负转换多反应监测(+/-)MRM 技术下首次同时检测到生物碱。考察了三种不同的色谱柱,样品在 Waters ACQUITY UPLC HSS T3(50×2.1mm(2),1.8μm)色谱柱上仅用 8min 即可用乙腈和甲酸-水溶液作为流动相,以 0.2mL/min 的流速分离。所有校准曲线在测试范围内均表现出良好的线性(r>0.999)。所建立的方法具有良好的灵敏度、日内和日间精密度、重现性和提取回收率。该方法成功应用于不同来源和不同收获期马齿苋中 8 种生物碱的测定。该方法也为其他复杂体系中生物碱的提取和测定提供了参考。

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