| 固相萃取/超高效液相色谱－三重四极杆质谱法测定人参、人参叶与人参花中10种人参皂苷含量 |
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| 基金项目:第四次全国中药资源普查项目（2017-152-009） |
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| 中文摘要:该文建立了超高效液相色谱－三重四极杆质谱测定人参、人参叶和人参花中10种主要人参皂苷的方法。采用Alumina－N/XAD-2 SPE Cartridge复合固相萃取柱净化样品，通过Hypersil Gold C18色谱柱（100 mm × 2.1 mm，1.9 μm），以5 mmol/L乙酸铵溶液（含0.1%甲酸）和乙腈为流动相进行分离，在电喷雾离子源负离子模式下，以多反应监测方式（MRM）检测。结果表明，10 种人参皂苷在5 ~ 2 500 ng/mL质量浓度范围内具有很好的线性关系，相关系数（r）均不小于0.998 0，检出限和定量下限分别为0.25 ~ 2.5 mg/kg和0.75 ~ 7.5 mg/kg。以人参叶为典型样品，在不同浓度加标水平下的平均回收率为87.3% ~ 110%，相对标准偏差（RSD）为1.4% ~ 9.3%。对不同批次的人参、人参叶和人参花检测结果表明，人参叶、人参花含有与人参相似的人参皂苷成分，且部分人参皂苷单体和10种主要人参皂苷总量远大于人参根部。该方法净化效果好，灵敏度高，重复性好，为人参资源的综合评价和全面控制提供了可靠的检测方法，同时为人参资源的开发和利用提供了基础资料。 |
| 中文关键词:人参皂苷 超高效液相色谱－三重四极杆质谱 固相萃取 人参叶 人参花 |
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| Determination of Ten Ginsenosides in Roots， Leaves and Flowers Buds of Panaxginseng by Solid Phase Extraction/Ultra Performance Liquid Chromatography－Triple Quadrupole Mass Spectrometry |
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| Abstract:A new method based on solid phase extraction/ultra performance liquid chromatography－triple quadrupole mass spectrometry was developed for the determination of ten ginsenosides in roots， leaves and flowers buds of panax ginseng. Firstly， the fragmentation process of the target compounds was determined by analyzing the fragments produced from the ionized lysis of ginsenosides under the negative ion mode of electrospray ion source（ESI－）. Then， the conditions of mass spectrometry and chromatography for the effective separation of 10 ginsenosides were optimized. Meanwhile， an Alumina－N/XAD-2 SPE cartridge composite solid phase extraction column was chosed as the pre-treatment purification column in this study， and XAD－2 macroporous adsorption resin and neutral alumina were also selected as the purification column materials. The principle of this research was based on the molecular exclusion effect of XAD－2 macroporous adsorption resin， which was liable to elute carbohydrates， proteins and organic acids in the sample， while the pigments and flavonoids in the sample were adsorbed by the neutral alumina. Therefore， the ginsenosides were able to further enriched and purified. Finally， the ginsenosides were separated on a Hypersil Gold C18 chromatographic column（100 mm × 2.1 mm， 1.9 μm） using 5 mmol/L ammonium acetate solution containing 0.1% formic acid and acetonitrile as the mobile phases. Furthermore， the ginsenosides were detected with electrospray ionization in negative ion mode under multiple reaction monitoring（MRM） mode. Results showed that there were good linear relationships for ten ginsenosides in the concentration range of 5－2 500 ng/mL， with their correlation coefficients（r） not less than 0.998 0. The limits of detection and limits of quantitation were in the ranges of 0.25－2.5 mg/kg and 0.75－7.5 mg/kg， respectively. For a typical sample of ginseng leaves， the average recoveries at different spiked levels ranged from 87.3% to 110%， with relative standard deviations（RSD） of 1.4%－9.3%. However， the results of different batches of ginseng， ginseng leaves and ginseng flowers showed that the ginsenoside components in leaves and flowers were similar to those in root， while the total contents of some ginsenoside monomers and ten main ginsenosides were more than those in the ginseng root. Overall， the results demonstrated that the proposed method was sensitive and accurate， and was suitable for the ginsenosides quantification in ginseng plants. The method could be applied to the content determination and quality control of ginseng， ginseng flowers and ginseng leaves， and provides a certain basis for the rational development and utilization of ginseng resources. |
| Key Words:ginsenosides ultra performance liquid chromatography－triple quadrupole mass spectrometry solid phase extraction ginseng leaves ginseng flowers |
| 引用本文：陈树东，胡文军，孔祥词，冯 锐，梁土金，崔媛媛，钟满霞.固相萃取/超高效液相色谱－三重四极杆质谱法测定人参、人参叶与人参花中10种人参皂苷含量[J].分析测试学报,2021,40(9):1348-1354. |
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