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HPTLC method for the simultaneous determination of six bioactive terpenoids in Putranjiva roxburghii Wall.
JPC - Journal of Planar Chromatography - Modern TLC ( IF 1.6 ) Pub Date : 2020-09-07 , DOI: 10.1007/s00764-020-00047-8
Sonali Mishra , Ramdas , Namita Gupta , Karuna Shanker

High-throughput and sensitive determination of triterpenoids is challenging by high-performance liquid chromatographic methods due to their non-chromophoric nature, lipophilic properties, and sequential run. The present study demonstrates the development of a validated high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination of bioactive terpenoids in the bark of Putranjiva roxburghii with uncertainty measurement to fulfill the technical requirement of ISO 17025:2017. Optimum separation of friedelin (1), methylputranjate (2), putrone (3), roxburghonic acid (4), putranjivadione (5), and roxburghonol (6) was achieved on silica gel 60 F254 plates using n-hexane–ethyl acetate (90:10, v/v). The sensitive estimation of targeted terpenoids was achieved by screening 15 different post-chromatographic derivatization reagents. The method was validated as per the ICH guidelines. Additionally, an uncertainty measurement for reliable and accurate determination was established following EURACHEM/CITAC guide CG-4 statistical procedure. The expanded uncertainty of terpenoids (16) measurement in P. roxburghii bark was in the range of 0.44–2.17%, which confirmed that at a confidence level of 95%, the unknown true value was within ± 5% range of the measured value. The compound methylputranjate showed the minimum uncertainty (0.4424), while putranjivadione showed the maximum uncertainty (2.1722). This is the first validated HPTLC method with new derivatization reagent providing the simultaneous, sensitive, and high-throughput analysis of six bioactive triterpenes in the bark of P. roxburghii with defined traceability and accuracy profile.



中文翻译:

HPTLC方法可同时测定Putranjiva roxburghii墙中的6种生物活性萜类化合物。

由于高效液相色谱方法的非生色性质,亲脂性和顺序运行,因此高效液相色谱法对三萜类化合物的高通量和灵敏测定具有挑战性。本研究证明了一种经验证的高性能薄层色谱法(HPTLC)的发展,该方法可同时测定普特兰吉瓦·罗克斯(Putranjiva roxburghii)树皮中的生物活性萜类化合物,并进行不确定度测量以满足ISO 17025:2017的技术要求。最佳分离弗里德林(1),甲基putranjate (2),putrone(3),roxburghonic acid(4),putranjivadione(5)和roxburghonol(6))中的溶液在硅胶上取得60°F 254使用板己烷-乙酸乙酯(90:10,体积/体积)。通过筛选15种不同的色谱分离后衍生试剂,可对目标萜类化合物进行灵敏估计。该方法已按照ICH指南进行了验证。此外,根据EURACHEM / CITAC指南CG-4统计程序建立了用于可靠和准确确定的不确定度测量。萜类化合物的扩展不确定度(1 - 6)测量在P.莲树皮在0.44–2.17%的范围内,这证实了在95%的置信度下,未知真实值在测量值的±5%范围内。复方甲普兰酯的不确定度最小(0.4424),而普兰吉瓦二酮的不确定度最大(2.1722)。这是第一种经过验证的HPTLC方法,使用新的衍生化试剂可对罗氏疟原虫树皮中的六个生物活性三萜进行同时,灵敏和高通量分析,并具有确定的可追溯性和准确性。

更新日期:2020-09-08
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