| 固相萃取-超高效液相色谱-串联质谱法检测保健食品中9种人参皂苷 |
| |
| 引用本文： | 陈树东,冯锐,林晓佳,梁土金,何秋婷. 固相萃取-超高效液相色谱-串联质谱法检测保健食品中9种人参皂苷[J]. 色谱, 2021, 39(5): 526-533. DOI: 10.3724/SP.J.1123.2020.04028 |
| |
| 作者姓名： | 陈树东 冯锐 林晓佳 梁土金 何秋婷 |
| |
| 作者单位： | 1.广东省中药研究所, 广东 广州 5106402.广东医科大学, 广东 东莞 5238083.广州检测认证集团有限公司, 广东 广州 511447 |
| |
| 摘 要： | 建立了以固相萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测保健食品中9种原人参二醇型和原人参三醇型人参皂苷的方法.保健食品中人参皂苷经过提取后,通过Alumina-N/XAD-2 SPE柱净化,在Hypersil Gold C18色谱柱(100 mm×2.1 mm,1.9μm)上分离,利用乙酸铵溶液(...
|
| 关 键 词： | 超高效液相色谱-串联质谱 固相萃取 人参皂苷 保健食品 |
| 收稿时间： | 2020-06-28 |
Determination of nine ginsenosides in health foods by solid extraction phase-ultra performance liquid chromatography-tandem mass spectrometry |
| |
| CHEN Shudong,FENG Rui,LIN Xiaojia,LIANG Tujin,HE Qiuting. Determination of nine ginsenosides in health foods by solid extraction phase-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese journal of chromatography, 2021, 39(5): 526-533. DOI: 10.3724/SP.J.1123.2020.04028 |
| |
| Authors: | CHEN Shudong FENG Rui LIN Xiaojia LIANG Tujin HE Qiuting |
| |
| Affiliation: | 1. Guangdong Institute of Traditional Chinese Medicine, Guangzhou 510640, China2. Guangdong Medical University, Dongguan 523808, China3. Guangzhou Inspection Testing and Certification Group Co., Ltd., Guangzhou 511447, China |
| |
| Abstract: | Ginsenosides are the main active compounds of ginseng, American ginseng and Panax notoginseng. They have certain pharmacological effects on the cardiovascular, immune and central nervous systems. Most ginsenosides are naturally classified as protopanaxatriol (PPT), protopanaxadiol (PPD), and oleanolic acid (OA) according to their aglycone skeletons. The nine main ginsenosides are Rb1, Rb2, Rb3, Rc, Rd, Re, Rf, Rg1 and Rg2. Accurate quantification of ginsenosides is imperative because they are the characteristic components and quality evaluation indicators of health foods. A new method based on solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) was developed for the determination of the nine ginsenosides in health foods. First, the pretreatment conditions were optimized. With the aim of purifying the samples and removing impurities, SPE cartridges with different packing materials, such as Alumina-N/XAD-2 SPE Cartridge, C18 and HLB were investigated. Based on the purification efficiencies, recoveries and other factors, the Alumina-N/XAD-2 SPE cartridge composite SPE column was selected as the pretreatment purification column. The eluents were then optimized. When water was used as the eluent, the ginsenosides could remain adsorbed on the SPE column, and could not be eluted down with other water-soluble substances. By increasing the proportion of ethanol in the eluent, the ginsenoside adsorbed on the filler of the SPE column could be gradually eluted. When the proportion of ethanol in the eluent reached 70%, the ginsenosides could be completely eluted. The effects of different volumes of 70% ethanol elution solvent (5-30 mL) on the extraction efficiencies of ginsenosides were also investigated. The results showed that when the volume of the elution solvent reached 20 mL, the ginsenosides were completely eluted. Then, the chromatographic conditions and MS parameters were optimized. By examining the ionization cracking of ginsenosides, the quasi-molecular ions and corresponding fragment ions in ginsenoside primary MS were determined. After optimizing the chromatographic conditions and MS parameters, not only the sensitivity of the method was improved, but also the isomers Rb2, Rb3 and Rc with the same quasi-molecular ions and the corresponding fragment ions were completely separated. Good separation was achieved for the nine ginsenosides, thus meeting the requirements for accurate quantification. Finally, chromatographic separation was achieved on a Hypersil Gold C18 column (100 mm×2.1 mm, 1.9 μm) under linear gradient elution using a 5 mmol/L ammonium acetate solution (with 0.1% formic acid) and acetonitrile as the mobile phases. The nine ginsenosides were detected using a triple quadrupole MS detector under ESI - and multiple reaction monitoring (MRM) modes, and quantified by the external standard method. The nine ginsenosides showed a strong positive linear correlation (r 2>0.9950) in the range of 0.005-0.5 μg/mL. The sample recoveries and the corresponding relative standard deviations (RSDs) were 81.1%-114.2% and 0.4%-8.0% (n=6), respectively. Eleven batches of health foods on the market, among which six batches contained ginseng, American ginseng or Panax notoginseng ingredients, were analyzed by the developed method, and the ginsenosides were detected. The total ginsenosides contents were close to those mentioned on the label. However, the nine ginsenosides were detected in one batch of health food, whose label did not indicated ginseng, American ginseng or Panax notoginseng. The nine ginsenosides were not detected in the remaining batches of health foods.The health food extract was directly loaded and purified without any complex pretreatment. The UPLC⁃MS/MS method, not only helped shorten the analysis time, but also accurate quantification of low ginsenoside contents in complex matrix samples. The developed method is simple and rapid, with high throughput, thus being suitable for the quantitative analysis of the nine ginsenosides in health foods. |
| |
| Keywords: | ultra performance liquid chromatography?tandem mass spectrometry (UPLC MS/MS) solid phase extraction (SPE) ginsenosides health foods |
|
| 点击此处可从《色谱》浏览原始摘要信息 |
|
点击此处可从《色谱》下载全文 |
|
