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一种使用超高效液相色谱-紫外-质谱联用技术对南非叶属植物、相关属以及膳食补充剂进行化学指纹图谱分析的快速方法。

A rapid method for chemical fingerprint analysis of Hoodia species, related genera, and dietary supplements using UPLC-UV-MS.

作者信息

Avula Bharathi, Wang Yan-Hong, Pawar Rahul S, Shukla Yatin J, Smillie Troy J, Khan Ikhlas A

机构信息

National Center for Natural Products Research, Research Institute of Pharmaceutical Sciences, The University of Mississippi, University, MS 38677, USA.

出版信息

J Pharm Biomed Anal. 2008 Nov 4;48(3):722-31. doi: 10.1016/j.jpba.2008.07.005. Epub 2008 Jul 15.

Abstract

Recently, ultra-performance liquid chromatography (UPLC) has proven to be one of the most promising developments in the area of high-speed chromatographic separations with increased sensitivity and resolution. In this work, a reverse phase chromatographic method was developed using UPLC for the chemical fingerprint analysis of 12 hoodigosides, related genera and dietary supplements. The method is also used for the quantification of P57 in Hoodia species and dietary supplements that claim to contain Hoodia. The analysis was performed on a Waters Acquity UPLC system with an Acquity UPLC BEH C18 column (100 mm x 2.1mm I.D., 1.7 microm) and a gradient elution of water and acetonitrile, both containing 0.05% formic acid with a run time of 15 min. The calibration curve of P57 showed good linearity (r(2)>0.999) within the established range (1-100 microg/mL). The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.3 and 0.9 microg/mL, respectively. The RSD for intra- and inter-day were less than 3.0%, and the recovery efficiency as 97-103%. LC-mass spectrometry coupled with electrospray ionization (ESI) interface method is described for the identification of P57. The developed method was successfully applied to the identification of 12 oxypregnane glycosides in four different species of Hoodia, 23 related genera and 35 dietary supplements that claim to contain H. gordonii. The UPLC profiles of various plant samples were compared for the presence of oxypregnane glycosides. Different sample matrices were successfully analyzed, providing the wide range of applicability of this method, including gels, capsules, tablets, sprays, tea bags, snack bars, powders and juices.

摘要

最近,超高效液相色谱法(UPLC)已被证明是高速色谱分离领域最具前景的发展之一,具有更高的灵敏度和分辨率。在本研究中,开发了一种使用UPLC的反相色谱方法,用于对12种蝴蝶亚科苷、相关属和膳食补充剂进行化学指纹图谱分析。该方法还用于定量分析蝴蝶亚科植物及声称含有蝴蝶亚科成分的膳食补充剂中的P57。分析在Waters Acquity UPLC系统上进行,使用Acquity UPLC BEH C18柱(100 mm×2.1mm内径,1.7微米),以水和乙腈进行梯度洗脱,二者均含有0.05%甲酸,运行时间为15分钟。P57的校准曲线在设定范围(1 - 100微克/毫升)内显示出良好的线性(r(2)>0.999)。检测限(LOD)和定量限(LOQ)分别为0.3和0.9微克/毫升。日内和日间的相对标准偏差(RSD)均小于3.0%,回收率为97 - 103%。描述了采用电喷雾电离(ESI)接口的液相色谱 - 质谱联用方法来鉴定P57。所开发的方法成功应用于鉴定四种不同蝴蝶亚科植物、23个相关属以及35种声称含有蝴蝶亚科成分的膳食补充剂中的12种氧代孕烷糖苷。比较了各种植物样品的UPLC图谱中氧代孕烷糖苷的存在情况。成功分析了不同的样品基质,证明了该方法具有广泛的适用性,包括凝胶、胶囊、片剂、喷雾剂、茶包、能量棒、粉末和果汁。

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