PK/PD and Toxicology Division, CSIR-Indian Institute of Integrative Medicine, Canal Road, Jammu, India.
Daru. 2013 Jan 29;21(1):11. doi: 10.1186/2008-2231-21-11.
A specific and sensitive UPLC-qTOF-MS/MS method has been developed for the simultaneous determination of curcuminoids. These Curcuminoids comprises of curcumin, a principal curcuminoid and other two namely, demethoxycurcumin, and bisdemethoxycurcumin obtained from rhizomes of Curcuma longa an ancient Indian curry spice turmeric, family (Zingiberaceae).
These analytes were separated on a reverse phase C18 column by using a mobile phase of acetonitrile: 5% acetonitrile in water with 0.07% acetic acid (75:25 v/v), flow rate of 100 μL/min was maintained. The qTOF-MS was operated under multiple reaction monitoring (MRM) mode using electro-spray ionization (ESI) technique with positive ion polarity. The major product ions in the positive mode for curcuminoids were at m/z 369.1066, 339.1023 and 309.0214 respectively. The recovery of the analytes from mouse plasma was optimized using solid phase extraction technique.
The total run time was 5 min and the peaks of the compounds, bisdemethoxycurcumin, demethoxycurcumin and curcumin occurred at 2.06, 2.23 and 2.40 min respectively. The calibration curves of bisdemethoxycurcumin, demethoxycurcumin and curcumin were linear over the concentration range of 2-1000 ng/mL (r2, 0.9951), 2-1000 ng/mL (r2, 0.9970) and 2-1000 ng/mL (r2, 0.9906) respectively.Intra-assay and inter-assay accuracy in terms of % bias for curcumin was in between -7.95to +6.21, and -7.03 to + 6.34; for demethoxycurcumin was -6.72 to +6.34, and -7.86 to +6.74 and for bisdesmetoxycurcumin was -8.23 to +6.37 and -8.47 to +7.81. The lower limit of quantitation for curcumin, demethoxycurcumin and bisdemethoxycurcumin was 2.0 ng/mL. Analytes were stable under various conditions (in autosampler, during freeze-thaw, at room temperature, and under deep-freeze conditions). This validated method was used during pharmacokinetic studies of curcumin in the mouse plasma.
A specific, accurate and precise UPLC-qTOF-MS/MS method for the determination of curcumin, demethoxycurcumin and bisdemethoxycurcumin both individually and simultaneously was optimized.
已经开发出一种特定且灵敏的 UPLC-qTOF-MS/MS 方法来同时测定姜黄素类化合物。这些姜黄素类化合物包括姜黄素，这是主要的姜黄素类化合物，以及另外两种分别是脱甲氧基姜黄素和双脱甲氧基姜黄素，它们是从姜黄的根茎中获得的，姜黄是一种古老的印度咖喱香料姜黄，属于姜科（Zingiberaceae）。
这些分析物在反相 C18 柱上分离，使用乙腈：5%乙腈在水中含 0.07%乙酸（75:25 v/v）的流动相，流速为 100 μL/min。qTOF-MS 采用电喷雾电离（ESI）技术在正离子极性下以多反应监测（MRM）模式运行。姜黄素类化合物在正模式下的主要产物离子的质荷比分别为 369.1066、339.1023 和 309.0214。使用固相萃取技术优化了分析物从小鼠血浆中的回收率。
总运行时间为 5 分钟，化合物双脱甲氧基姜黄素、脱甲氧基姜黄素和姜黄素的峰分别出现在 2.06、2.23 和 2.40 分钟。双脱甲氧基姜黄素、脱甲氧基姜黄素和姜黄素的校准曲线在 2-1000 ng/mL（r2，0.9951）、2-1000 ng/mL（r2，0.9970）和 2-1000 ng/mL（r2，0.9906）范围内呈线性。姜黄素的日内和日间准确度（以%偏倚表示）分别在-7.95 至+6.21 和-7.03 至+6.34 之间；脱甲氧基姜黄素分别在-6.72 至+6.34 和-7.86 至+6.74 之间；双脱甲氧基姜黄素分别在-8.23 至+6.37 和-8.47 至+7.81 之间。姜黄素、脱甲氧基姜黄素和双脱甲氧基姜黄素的定量下限均为 2.0 ng/mL。分析物在各种条件下（在自动进样器中、在冻融期间、在室温下和在深冻条件下）均稳定。该经过验证的方法用于在小鼠血浆中进行姜黄素的药代动力学研究。
优化了一种特定、准确和精确的 UPLC-qTOF-MS/MS 方法，用于同时单独和同时测定姜黄素、脱甲氧基姜黄素和双脱甲氧基姜黄素。
