Chemical fingerprint analysis and quantitative determination of steroidal compounds from Dioscorea villosa, Dioscorea species and dietary supplements using UHPLC-ELSD.
Chemical fingerprint analysis and quantitative determination of steroidal compounds from Dioscorea villosa, Dioscorea species and dietary supplements using UHPLC-ELSD.
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DOI：
10.1002/bmc.3019
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发表时间：
2014-02
影响因子：
1.8
通讯作者：
Khan, Ikhlas A.
中科院分区：
文献类型：
--
作者：
Avula, Bharathi;Wang, Yan-Hong;Ali, Zulfiqar;Smillie, Troy J.;Khan, Ikhlas A.
采用超高效液相色谱法(UHPLC) -蒸发光散射法（ELS）测定了不同薯蓣种属根茎和块茎及含有薯蓣的膳食补充剂中甾体皂苷和薯蓣皂苷元的含量。分析采用Acquity UPLC™系统，UPLC™BEH Shield RP18色谱柱，采用水和乙腈梯度洗脱。由于甾体皂苷的紫外吸收较低，采用蒸发光散射法对其进行检测。该方法可在15 min内分离出12个化合物，检出限为5 ~ 12 μg/mL，进样量为2μL。验证了分析方法的线性度、重复性、准确度、检出限和定量限。日内、日间实验的相对标准偏差（RSD）均小于3.1%，回收率为97 ~ 101%。干燥植物原料和固体商业制剂的标准化合物总含量分别为每日摄入量0.01 ~ 14.5%和0.9 ~ 28.6 mg。采用四极杆质谱分析仪和ESI源的uhplc -质谱法仅用于确认各种皂苷的身份。该方法简便、快速，特别适用于商品的质量控制分析。
Ultra high-performance liquid chromatography (UHPLC) with evaporative light scattering (ELS) detection was used for the quantification of steroidal saponins and diosgenin from the rhizomes or tubers of various Dioscorea species and dietary supplements that were purported to contain Dioscorea. The analysis was performed on an Acquity UPLC™ system with an UPLC™ BEH Shield RP18 column using a gradient elution with water and acetonitrile. Due to their low UV absorption, the steroidal saponins were observed by evaporative light scattering detection. The twelve compounds could be separated within 15 minutes using the developed UHPLC method with detection limits of 5–12 μg/mL with 2μL injection volume. The analytical method was validated for linearity, repeatability, accuracy, limits of detection (LOD) and limits of quantification (LOQ). The Relative Standard Deviations (RSD) for intra- and inter-day experiments were less than 3.1 %, and the recovery efficiency was 97–101 %. The total content of standard compounds was found to be in the range from 0.01–14.5% and 0.9–28.6 mg daily intake for dry plant materials and solid commercial preparations, respectively. UHPLC-mass spectrometry with a quadrupole mass analyzer and ESI source was used only for confirmation of the identity of the various saponins. The developed method is simple, rapid and especially suitable for quality control analysis of commercial products.
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DOI：
10.5962/bhl.part.19785
发表时间：
1989-01-01
期刊：
JOURNAL OF THE ARNOLD ARBORETUM
影响因子：
--
作者：
ALSHEHBAZ, IA;SCHUBERT, BG
通讯作者：
SCHUBERT, BG
影响因子：
8.8
作者：
Lin, Jau-Tien;Yang, Deng-Jye
通讯作者：
Yang, Deng-Jye
影响因子：
6.2
作者：
Liu, Chun-Zhao;Zhou, Hua-Ying;Yan, Qiong
通讯作者：
Yan, Qiong
影响因子：
3.1
作者：
Ali, Zulfiqar;Smillie, Troy J.;Khan, Ikhlas A.
通讯作者：
Khan, Ikhlas A.
影响因子：
2.3
作者：
Li, R;Zhou, Y;Ding, LS
通讯作者：
Ding, LS