反相高效液相色谱法同时测定参苓白术颗粒中白术内酯Ⅱ及白术内酯.docVIP

反相高效液相色谱法同时测定参苓白术颗粒中白术内酯Ⅱ及白术内酯 　作者：葛建，楼纪东，林芳，黄丽红，姜威，李明揆，卢秀莲 【摘要】 　　目的建立一种同时测定白术内酯Ⅱ和白术内酯Ⅲ的高效液相色谱检测方法，并分析中成药参苓白术颗粒中白术内酯Ⅱ和白术内酯Ⅲ的含量。方法样品采用液-液萃取，以乙腈-水（50∶50）为流动相，流速1.0 ml· min-1，采用SHIMADZU ODS柱（150 mm×4.6 mm; 5 μm）色谱柱分离；检测波长220 nm。结果标准曲线线性范围为0.5～50.0 μg·ml-1，线性关系良好(rgt;0.99)，定量限为0.5 μg/ml，回收率98%以上，方法的稳定性、重复性和精密度均较好（RSDlt;3%）。结论该法操作简便、快速、灵敏、准确，已经成功地用于中成药参苓白术颗粒中白术内酯Ⅱ和白术内酯Ⅲ的含量测定。 【关键词】 白术内酯Ⅱ 白术内酯Ⅲ 高效液相色谱-紫外检测法 参苓白术颗粒 　　Abstract：ObjectiveTo develop an HPLC-UV method for the simultaneous determination of atractylenolide II and III and to detect the content of atractylenolide II and III in Chinese medicinal preparation.MethodsAfter a simple liquid-liquid extraction, atractylenolide II and III were separated on SHIMADZU C18 column(4.6 mm×150 mm, 5 μm) and detected by UV spectrometry. The detection wavelength was set at 220 nm. The mobile phase consisted of acetonitrile-water (50∶50) at a flow rate of 1.0 ml·min-1. The content of atractylenolide II and III in Chinese medicinal preparation(Shenling Baizhu Granule) was simultaneously determined by the method above after simple liquid-liquid extraction.ResultsThe linear calibration curves were obtained in the concentration range of 0.5～50.0 μg·ml-1(rgt;0.99). The lower limit of quantification was 0.5 μg·ml-1. The recoveries were more than 98.0%, and the stability, repeatability and precision of the method were all better in all cases（RSDlt;3%）. ConclusionThe RP-HPLC method is specific, simple, sensitive and accurate. And this method was successfuly applied to simultaneously quantitate atractylenolide II and III in Chinese medicinal preparation (Shenling Baizhu Granule). 　　Key words：Atractylenolide II; Atractylenolide III; RP-HPLC; Shenling Baizhu Granule 　　参苓白术颗粒由人参、白术（炒）、茯苓等中药组成，具有补脾胃，益肺气的功效，用于脾胃虚弱，食少便溏，气短咳嗽，肢倦乏力［1］。白术为本方中重要组成部分，白术为菊科植物白术Atractylodes macrocephala Koidz.的干燥根茎，为常用大宗药材，著名的“浙八味”之一［2］。其味苦、甘,性温,归脾胃经,功能健脾益气、燥湿利水、止汗、安胎,为补益类补气药［3］。白术内酯Ⅱ和白术内酯Ⅲ为白术中的有效成分，该类物质具有抗炎、抗肿瘤作用［4］。此外该类成分还具有调节胃肠道功能和促进营养物质吸引的功能［5］。有学者采用了人参皂苷［6］作为检测指标来对