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Validated Reverse Phase-High-Performance Liquid Chromatography Method for Estimation of Fisetin in Self-Nanoemulsifying Drug Delivery System.
ASSAY and Drug Development Technologies ( IF 1.6 ) Pub Date : 2020-09-16 , DOI: 10.1089/adt.2020.983
Rajan Kumar 1 , Rakesh Kumar 1 , Rubiya Khursheed 1 , Ankit Awasthi 1 , Arya Kadukkattil Ramanunny 1 , Jaskiran Kaur 1 , Navneet Khurana 1 , Sachin Kumar Singh 1 , Shelly Khurana 2 , Narendra Kumar Pandey 1 , Bhupinder Kapoor 1 , Neha Sharma 1
Affiliation  

Fisetin (FS) is a polyphenolic phytoconstituent reported to have various pharmacological activities such as antioxidant, antiparkinsonian, and antidepressant. An analytical method was developed and validated for the estimation of FS by ultrafast liquid chromatography using C-18 reverse phase column. Acetonitrile and orthophosphoric acid (0.2% v/v) in the ratio of 30:70 v/v was used as mobile phase. Flow rate was set at 1 mL/min. Chromatogram of FS was detected at wavelength of 362 nm. Retention time for FS was found to be 7.06 min. The developed method was found to be linear in the range of 2–10 μg/mL with regression coefficient of 0.9985. The method was validated as per the International Conference on Harmonization (ICH) Q2 (R1) guidelines. The percentage recovery was in the range of 95%–105%, which indicated the accuracy of the method. The percentage relative standard deviation (RSD) was found to be <2%, which indicates the precision of the method. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.46 and 1.41 μg/mL, respectively. The developed method was found to be robust as there was no significant change in response with change in flow rate, ratio of mobile phase, and pH. The method was successfully applied for estimation of drug loading and drug release from self-nanoemulsifying drug delivery system (SNEDDS). The % drug loading of FS in prepared liquid SNEDDS formulation was found to be 101.95%. The results of dissolution studies indicated 67.78% FS release in water at the end of 60 min.

中文翻译:

用于估计自纳米乳化给药系统中非瑟酮的有效反相高效液相色谱方法。

Fisetin (FS) 是一种多酚植物成分,据报道具有多种药理活性,如抗氧化、抗帕金森病和抗抑郁药。开发并验证了使用 C-18 反相柱通过超快速液相色谱法估算 FS 的分析方法。使用比例为 30:70 v/v 的乙腈和正磷酸 (0.2% v/v) 作为流动相。流速设定为 1 mL/min。在 362 nm 波长处检测到 FS 的色谱图。发现 FS 的保留时间为 7.06 分钟。发现开发的方法在 2–10 μg/mL 范围内呈线性,回归系数为 0.9985。该方法已根据国际协调会议 (ICH) Q2 (R1) 指南进行验证。回收率在 95%~105% 范围内,表明该方法的准确性。发现百分比相对标准偏差 (RSD) < 2%,表明该方法的精密度。检测限 (LOD) 和定量限 (LOQ) 分别为 0.46 和 1.41 μg/mL。发现开发的方法是稳健的,因为随着流速、流动相比率和 pH 值的变化,响应没有显着变化。该方法已成功应用于估计自纳米乳化给药系统(SNEDDS)的载药量和药物释放量。发现所制备的液体 SNEDDS 制剂中 FS 的药物负载百分比为 101.95%。溶解研究的结果表明在 60 分钟结束时 67.78% FS 在水中释放。检测限 (LOD) 和定量限 (LOQ) 分别为 0.46 和 1.41 μg/mL。发现开发的方法是稳健的,因为随着流速、流动相比率和 pH 值的变化,响应没有显着变化。该方法已成功应用于估计自纳米乳化给药系统(SNEDDS)的载药量和药物释放量。发现所制备的液体 SNEDDS 制剂中 FS 的药物负载百分比为 101.95%。溶解研究的结果表明在 60 分钟结束时 67.78% FS 在水中释放。检测限 (LOD) 和定量限 (LOQ) 分别为 0.46 和 1.41 μg/mL。发现开发的方法是稳健的,因为随着流速、流动相比率和 pH 值的变化,响应没有显着变化。该方法已成功应用于估计自纳米乳化给药系统(SNEDDS)的载药量和药物释放量。发现所制备的液体 SNEDDS 制剂中 FS 的药物负载百分比为 101.95%。溶解研究的结果表明在 60 分钟结束时 67.78% FS 在水中释放。该方法已成功应用于估计自纳米乳化给药系统(SNEDDS)的载药量和药物释放量。发现所制备的液体 SNEDDS 制剂中 FS 的药物负载百分比为 101.95%。溶解研究的结果表明在 60 分钟结束时 67.78% FS 在水中释放。该方法已成功应用于估计自纳米乳化给药系统(SNEDDS)的载药量和药物释放量。发现所制备的液体 SNEDDS 制剂中 FS 的药物负载百分比为 101.95%。溶解研究的结果表明在 60 分钟结束时 67.78% FS 在水中释放。
更新日期:2020-09-17
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