TY - JOUR AU - Ika, Marlina AU - Andalusia, Rizka AU - Supandi, Supandi AU - Harahap, Yahdiana PY - 2017/10/30 Y2 - 2024/03/29 TI - SIMULTANEOUS ANALYTICAL METHOD DEVELOPMENT OF 6-MERCAPTOPURINE AND 6-METHYLMERCAPTOPURINE IN DRIED BLOOD SPOT USING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY JF - International Journal of Applied Pharmaceutics JA - Int J App Pharm VL - 9 IS - 0 SE - Original Article(s) DO - 10.22159/ijap.2017.v9s1.80_87 UR - https://journals.innovareacademics.in/index.php/ijap/article/view/23335 SP - 168-171 AB - <p>Objective: 6-mercaptopurine (6-MP) is a chemotherapeutic agent in the antimetabolite class. It has to go through the metabolic pathway to form<br />6-methyl MP (6-MMP). This study aimed to obtain an optimum and validated method for the analysis of 6-MP and 6-MMP in dried blood spot (DBS)<br />samples simultaneously and to evaluate the potential for future drug concentration monitoring in DBS samples.<br />Methods: The quality control and calibration curves were made by spotting 40 μL blood on DBS paper and dried for 3 hrs. DBS papers were cut with a<br />diameter of 8 mm and extracted with acetonitrile-methanol (1:3) containing internal standard 5-fluorouracil (5-FU). Separation was performed with<br />waters acquity ultra performance liquid chromatography BEH C18 column of 1.7 μm (2.1×100 mm) with a mobile phase consisting of 0.1% formic<br />acid in water 0.1% formic acid in acetonitrile with gradient elution and a flow rate of 0.2 mL/minute. Mass detection was performed using Waters<br />Xevo TQD with positive electrospray ionization (ESI) for 6-MP and 6-MMP and negative ESI for 5-FU in the multiple reaction monitoring mode.<br />Results: The detection rates of 6-MP, 6-MMP, and 5-FU were 153.09&gt;119.09, 167.17&gt;126.03, and 129.09&gt;42.05, respectively. This method was linear<br />with the range at 26-1000 ng/mL for 6-MP and 13-500 ng/mL for 6-MMP with consecutive r≥0.998 and ≥0.999, respectively. The % relative error<br />value and % relative standard deviation for accuracy and precision of intraday and interday were not more than 15% and not more than 20% at the<br />lower limit of quantification concentration, respectively.<br />Conclusions: This method fulfilled the requirements of selectivity, linearity, carry over, and matrix effects referring to the European Medicines Agency<br />guidelines.</p> ER -