| 摘要: |
| 目的引入加速溶剂萃取(accelerated solvent extraction, ASE)技术,并结合HPLC-TOF/MS法同时测定重楼中6种甾体皂苷类成分的含量。方法加速溶剂萃取仪在120℃、1.17 MPa (1 700 psi)压力下,用70%的乙醇静态萃取样品6 min；6种重楼皂苷的含量用HPLC-TOF/MS同时测定,色谱柱: MGC18柱(3.0 mm×100 mm,3.0 μm)；流动相: 乙腈与0.1%(V/V)甲酸水,梯度洗脱；流速: 0.8 ml/min；柱温: 25℃；进样量: 3 μl；离子源: ESI正离子模式；雾化气压力: 275.85 kPa(40 psi)；干燥气流速: 10 L/min；干燥气温度: 350℃。结果重楼皂苷Ⅰ、重楼皂苷Ⅱ、重楼皂苷Ⅵ、重楼皂苷Ⅶ、薯蓣皂苷和纤细薯蓣皂苷的线性范围(μg/ml)分别为: 0.500 0~50.00(r=0.999 8)、0.422 3~42.23(r=0.999 7)、0.612 0~61.20(r=0.999 9)、0.714 0~71.40(r=0.999 5)、0.448 0~44.80(r=0.999 9)和0.436 0~43.60(r=0.999 7)；各成分的平均回收率(n=6)分别为98.9%、98.0%、102.5%、101.9%、103.1%和97.9%。结论该法溶剂消耗少、耗时短、便于自动化,可实现高通量分析,可用于重楼中皂苷类成分的含量测定。 |
| 关键词: 重楼 甾体皂苷 加速溶剂萃取 高效液相飞行时间质谱 |
| DOI：10.3724/SP.J.1008.2012.00549 |
| 投稿时间：2012-02-13修订日期：2012-03-19 |
| 基金项目: |
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| Simultaneous determination of 6 steroidal saponins in Paris Polyphylla by accelerated solvent extraction-HPLC-TOF/MS |
| WANG Ben-wei,ZHAO Liang,ZHANG Hai,LV Lei,LI Yue-yue,ZHANG Guo-qing﹡ |
(Department of Pharmacy, Eastern Hepatobiliary Hospital, Second Military Medical University, Shanghai 200438, China
*Corresponding author.) |
| Abstract: |
| ObjectiveTo introduce an accelerated solvent extraction (ASE) -HPLC-TOF/MS method for simultaneous determination of Polyphyllin Ⅰ, Polyphyllin Ⅱ, Polyphyllin Ⅵ, Polyphyllin Ⅶ, Dioscin and Gracillin in Paris Polyphylla. MethodsThe extraction was performed by ASE under the following conditions: extracting solvent 70% ethanol; extracting temperature 120℃; pressure 1.17 MPa (1 700 psi); and static time 6 min. The separation was carried out on a MGC18 column (3.0 mm×100 mm, 3.0 μm). Elution was done with a linear gradient mobile phase system consisting of 0.1% formic acid (V/V) water and acetonitrile. The flow rate was set at 0.8 ml/min, the sample injection volume was 3 μl, the column temperature was kept constant at 25℃, nebulizer gas pressure was 275.8 kPa (40 psi), drying gas flow rate was 10 L/min, and gas temperature was 350℃. ResultsThe calibration curves for Polyphyllin Ⅰ, Polyphyllin Ⅱ, Polyphyllin Ⅵ, Polyphyllin Ⅶ, Dioscin and Gracillin were linear within the range of 0.500 0-50.00 μg/ml (r=0.999 8), 0.422 3-42.23 μg/ml (r=0.999 7), 0.612 0-61.20 μg/ml (r=0.999 9), 0.714 0-71.40 μg/ml (r=0.999 5), 0.448 0-44.80 μg/ml (r=0.999 9) and 0.436 0-43.60 μg/ml (r=0.9997), respectively; and the average recoveries (n=6) were 98.9%, 98.0%, 102.5%, 101.9%, 103.1% and 97.9%, respectively. ConclusionThe introduced method is solvent-saving and time-saving; it can also be used for high-throughput analysis and determination of steroidal saponins in Paris Polyphylla. |
| Key words: Paris Polyphylla steroidal saponins accelerated solvent extraction HPLC-TOF/MS |
