Dr Reddy's Laboratories Ltd, Generics AR&D, Bachupalli, Qutubllapur, AP, India.
Drug Test Anal. 2010 Mar;2(3):107-12. doi: 10.1002/dta.112.
A selective, specific and sensitive ultra high pressure liquid chromatography (UHPLC) method was developed for determination of tacrolimus degradation products and tautomers in the preparation of pharmaceuticals. The chromatographic separation was performed on Waters ACQUITY UPLC system and BEH C₈ column using gradient elution of mobile phase A (90:10 v/v of 0.1% v/v triflouroacetic acid solution and Acetonitrile) and mobile phase B (90:10 v/v acetonitrile and water) at a flow rate of 0.6 mL min⁻¹. Ultraviolet detection was performed at 210 nm. Tacrolimus, tautomers and impurities were chromatographed with a total run time of 25 min. Calibration showed that the response of impurity was a linear function of concentration over the range 0.3-6 µg mL⁻¹ (r² ≥ 0.999) and the method was validated over this range for precision, intermediate precision, accuracy, linearity and specificity. For precision study, percentage relative standard deviation of each impurity was < 15% (n = 6). The method was found to be precise, accurate, linear and specific. The proposed method was successfully employed for estimation of tacrolimus impurities in pharmaceutical preparations.
建立了一种用于药物制备中测定他克莫司降解产物和互变异构体的选择性、特异性和灵敏的超高效液相色谱（UHPLC）方法。在 Waters ACQUITY UPLC 系统和 BEH C₈柱上，采用梯度洗脱，流动相 A（90:10 v/v 0.1% v/v 三氟乙酸溶液和乙腈）和流动相 B（90:10 v/v 乙腈和水），流速为 0.6 mL min⁻¹。在 210nm 处进行紫外检测。他克莫司、互变异构体和杂质的总运行时间为 25min。校准表明，杂质的响应是浓度在 0.3-6μg mL⁻¹范围内的线性函数（r²≥0.999），该方法在该范围内进行了精密度、中间精密度、准确度、线性和专属性验证。对于精密度研究，每个杂质的相对标准偏差百分比均小于 15%（n=6）。该方法精确、准确、线性和专属性良好。该方法成功用于估计药物制剂中他克莫司的杂质。
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