Hasnain M Saquib, Rao Shireen, Singh Manoj Kr, Vig Nitin, Singh Manish Kr, Budakoti Subodh Kr, Ansari Abdulla
Department of Pharmaceutical Chemistry, Seemanta Institute of Pharmaceutical Sciences, Orissa, India.
J Pharm Bioallied Sci. 2013 Jan;5(1):74-9. doi: 10.4103/0975-7406.106571.
For the determination of desloratadine (DES) and 3-OH desloratadine (3-OHD) in human plasma using deutrated desloratadine (DESD5) as internal standard (IS), a novel stability indicating liquid chromatography-tandem mass spectrometric method was developed and validated to support the clinical advancement.
The solid-phase extraction method used for sample preparation and calibration range was 100-11,000 pg/ml, for which a quadratic regression (1/x(2)) was best fitted. The blank plasma was screened and observed free from any endogenous interference.
The accuracy (% nominal) at low limit of quantification LLOQ level for DES and 3-OHD was 100.4% and 99.9% whereas precision (%CV) was 4.6 and 5.1%. They (DES and 3-OHD) were stable in human plasma after five freeze-thaw cycles, at room temperature for 23.8 hour, bench top stability for 6.4 hour.
This method fulfills all the regulatory requirements for selectivity, sensitivity, precision, accuracy, stability, goodness of fit, and ruggedness of the method for the determination of DES and 3-OHD in human plasma.
为了以氘代地氯雷他定（DESD5）作为内标（IS）测定人血浆中的地氯雷他定（DES）和3 - 羟基地氯雷他定（3 - OHD），开发并验证了一种新型的稳定性指示液相色谱 - 串联质谱法以支持临床研究进展。
用于样品制备的固相萃取方法，校准范围为100 - 11,000 pg/ml，对此二次回归（1/x²）拟合最佳。对空白血浆进行筛选并观察到无任何内源性干扰。
DES和3 - OHD在定量下限（LLOQ）水平的准确度（%标称值）分别为100.4%和99.9%，而精密度（%CV）分别为4.6和5.1%。它们（DES和3 - OHD）在人血浆中经过五次冻融循环后、在室温下23.8小时以及在台式稳定性条件下6.4小时均稳定。
该方法满足了测定人血浆中DES和3 - OHD的方法在选择性、灵敏度、精密度、准确度、稳定性、拟合优度和耐用性方面的所有监管要求。
