Chandu Babu Rao, Kanala Kanchanamala, Hwisa Nagiat T, Katakam Prakash, Khagga Mukkanti
Faculty of Pharmacy, University of Al-Zawia, Zawiya, Libya.
Springerplus. 2013 Apr 30;2(1):194. doi: 10.1186/2193-1801-2-194. Print 2013 Dec.
A bioequivalence study was proved of generic Febuxostat 80 mg tablets (T) in healthy volunteers.For this purpose, Authors developed a simple, sensitive, selective, rapid, rugged and reproducible liquid chromatography-tandem mass spectrometry method for the quantification of Febuxostat (FB) in human plasma using Febuxostat D7 (FBD7) as an internal standard (IS) was used. Chromatographic separation was performed on Ascentis Express C18 (50x4.6 mm, 3.5 μ) column. Mobile phase composed of 10 mM Ammonium formate: Acetonitrile (20:80 v/v), with 0.8 mL/min flow-rate. Drug and IS were extracted by Liquid- liquid extraction. FB and FBD7 were detected with proton adducts at m/z 317.1→261.1 and 324.2→262.1 in multiple reaction monitoring (MRM) positive mode respectively. The method was validated with the correlation coefficients of (r(2)) ≥ 0.9850 over a linear concentration range of 1.00-8000.00 ng/mL. This method demonstrated intra and inter-day precision within 2.64 to 3.88 and 2.76 to 8.44% and accuracy within 97.33 to 99.05 and 100.30 to 103.19% for FB. This method is successfully applied in the Bioequivalence study of 9 human volunteers.
一项关于80毫克非布司他仿制药片（T）在健康志愿者中的生物等效性研究得到了验证。为此，作者开发了一种简单、灵敏、选择性好、快速、耐用且可重现的液相色谱-串联质谱法，以非布司他D7（FBD7）作为内标（IS）来定量测定人血浆中的非布司他（FB）。色谱分离在Ascentis Express C18（50×4.6毫米，3.5微米）柱上进行。流动相由10毫摩尔甲酸铵：乙腈（20:80 v/v）组成，流速为0.8毫升/分钟。药物和内标通过液-液萃取进行提取。在多反应监测（MRM）正模式下，分别在m/z 317.1→261.1和324.2→262.1处检测到FB和FBD7的质子加合物。该方法在1.00 - 8000.00纳克/毫升的线性浓度范围内，相关系数（r(2)）≥0.9850，得到了验证。该方法对FB的日内和日间精密度分别在2.64%至3.88%和2.76%至8.44%之间，准确度分别在97.33%至99.05%和100.30%至103.19%之间。该方法已成功应用于9名人类志愿者的生物等效性研究。
