scholarly journals A Quantitative Method for the Measurement of Dried Blood Spot Amino Acids Using Ultra-Performance Liquid Chromatography

2016 ◽  
Vol 1 (3) ◽  
pp. 271-279 ◽  
Author(s):  
Kaitlyn Bloom ◽  
Gail Ditewig Meyers ◽  
Michael J. Bennett
Keyword(s):  
Amino Acids ◽  
Liquid Chromatography ◽  
Quantitative Method ◽  
Ultra Performance Liquid Chromatography ◽  
Dried Blood Spot ◽  
Blood Spot

scholarly journals VALIDATION OF 6-MERCAPTOPURINE AND 6-THIOGUANINE IN DRIED BLOOD SPOT BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

2018 ◽  
Vol 10 (1) ◽  
pp. 412
Author(s):  
Yahdiana Harahap ◽  
Cheputri Rahma Astrini ◽  
Herman Suryadi
Keyword(s):  
Liquid Chromatography ◽  
Formic Acid ◽  
High Performance ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Dried Blood Spot ◽  
European Medicines Agency ◽  
Tandem Mass ◽  
Liquid Chromatography Tandem Mass ◽  
Blood Spot

Objective: This study aimed to obtain an optimal and validated method of analyzing 6-mercaptopurine (6-MP) and 6-thioguanine (6-TG) simultaneouslyin dried blood spot samples using ultra high-performance liquid chromatography-tandem mass spectrometry.Method: Separation was performed with a 1.7-μm amide column, which had a mobile phase with a flow rate of 0.2 mL/min and comprised 0.2%formic acid in water, 0.1% formic acid in acetonitrile, and methanol with a gradient elution. Detection was performed using Waters Xevo TQD.Result: This method was linear with a range of 25–1000 ng/mL for 6-MP and 6-TG, with consecutive r values of ≥0.996 and ≥0.995, respectively. Theintra- and inter-day % difference value and coefficient of variation for the accuracy and precision were not more than 15% and 20%, respectively, ata concentration lower limit of quantitation.Conclusion: This method fulfilled the requirements of the European Medicines Agency guideline for validation.

scholarly journals Simultaneous Analysis of 6-Mercaptopurine, 6-Methylmercaptopurine, and 6-Thioguanosine-5’-monophosphate in Dried Blood Spot Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

2018 ◽  
Vol 18 (3) ◽  
pp. 544 ◽  
Author(s):  
Supandi Supandi ◽  
Yahdiana Harahap ◽  
Harmita Harmita ◽  
Rizka Andalusia
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Formic Acid ◽  
Ultra Performance Liquid Chromatography ◽  
Dried Blood Spot ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Blood Spot

6-Mercaptopurine is a chemotherapeutic agent of the antimetabolite class. This study aims to analyze simultaneous validation of 6-mercaptopurine (6-MP), 6-methylmercaptopurine (6-MMP), and 6-thioguanosine-5’-monophosphate (6-TGMP) in dried blood spot (DBS) using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). An accurate volume of 60 μL blood was spotted onto DBS-CAMAG paper and then extracted using methanol 90% (v/v) containing an internal standard of 5-fluorouracil (5-FU). Separation was performed using a Waters Acquity UPLC BEH AMIDA column 1.7 μm (2.1 x 100 mm) with a mobile phase mixture of 0.2% (v/v) formic acid in water−0.1% (v/v) formic acid in acetonitrile-methanol with gradient elution and flow rate of 0.2 mL/min. Mass detection was done using Waters Xevo TQD with positive electrospray ionization (ESI) for 6-MP, 6-MMP, 6-TGMP and negative ESI for 5-FU, in multiple reaction monitoring mode. Detection rates of 6-MP, 6-MMP, 6-TGMP and 5-FU were m/z 153.09 > 119.09; 167.17 > 126.03; 380.16 > 168.00); 129.09 > 42.05, respectively. This method is linear across the range 25.5–1020 ng/mL for 6-MP, 6-MMP and 6-TGMP. This method is valid for the in vitro simultaneous analysis of 6-MP, 6-MMP and 6-TGMP in DBS, based on European Medicine Agency guidelines.

scholarly journals SIMULTANEOUS ANALYTICAL METHOD DEVELOPMENT OF 6-MERCAPTOPURINE AND 6-METHYLMERCAPTOPURINE IN DRIED BLOOD SPOT USING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY

2017 ◽  
Vol 9 ◽  
pp. 168
Author(s):  
Marlina Ika ◽  
Rizka Andalusia ◽  
Supandi Supandi ◽  
Yahdiana Harahap
Keyword(s):  
Liquid Chromatography ◽  
Method Development ◽  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Dried Blood Spot ◽  
Mass Detection ◽  
Relative Standard ◽  
Blood Spot

Objective: 6-mercaptopurine (6-MP) is a chemotherapeutic agent in the antimetabolite class. It has to go through the metabolic pathway to form6-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)samples simultaneously and to evaluate the potential for future drug concentration monitoring in DBS samples.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 adiameter of 8 mm and extracted with acetonitrile-methanol (1:3) containing internal standard 5-fluorouracil (5-FU). Separation was performed withwaters acquity ultra performance liquid chromatography BEH C18 column of 1.7 μm (2.1×100 mm) with a mobile phase consisting of 0.1% formicacid 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 WatersXevo TQD with positive electrospray ionization (ESI) for 6-MP and 6-MMP and negative ESI for 5-FU in the multiple reaction monitoring mode.Results: The detection rates of 6-MP, 6-MMP, and 5-FU were 153.09>119.09, 167.17>126.03, and 129.09>42.05, respectively. This method was linearwith 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 errorvalue and % relative standard deviation for accuracy and precision of intraday and interday were not more than 15% and not more than 20% at thelower limit of quantification concentration, respectively.Conclusions: This method fulfilled the requirements of selectivity, linearity, carry over, and matrix effects referring to the European Medicines Agencyguidelines.

scholarly journals Identification of Auxin Metabolites in Brassicaceae by Ultra-Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry

Molecules ◽  
2019 ◽  
Vol 24 (14) ◽  
pp. 2615 ◽  
Author(s):  
Panagiota-Kyriaki Revelou ◽  
Maroula G. Kokotou ◽  
Violetta Constantinou-Kokotou
Keyword(s):  
Mass Spectrometry ◽  
Amino Acids ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Plant Extracts ◽  
High Resolution Mass Spectrometry ◽  
Ultra Performance Liquid Chromatography ◽  
Charge Ratio ◽  
High Resolution Mass ◽  
Resolution Mass

Auxins are signaling molecules involved in multiple stages of plant growth and development. The levels of the most important auxin, indole-3-acetic acid (IAA), are regulated by the formation of amide and ester conjugates with amino acids and sugars. In this work, IAA and IAA amide conjugates with amino acids bearing a free carboxylic group or a methyl ester group, along with some selected IAA metabolites, were studied in positive and negative electrospray ionization (ESI) modes, utilizing high-resolution mass spectrometry (HRMS) as a tool for their structural analysis. HRMS/MS spectra revealed the fragmentation patterns that enable us to identify IAA metabolites in plant extracts from eight vegetables of the Brassicaceae family using a fast and reliable ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-QToF-MS) method. The accurate m/z (mass to charge) ratio and abundance of the molecular and fragment ions of the studied compounds in plant extracts matched those obtained from commercially available or synthesized compounds and confirmed the presence of IAA metabolites.

Quantitation of sulfur-containing amino acids, homocysteine, methionine and cysteine in dried blood spot from newborn baby by HPLC-fluorescence detection

2014 ◽  
Vol 28 (6) ◽  
pp. 810-814 ◽  
Author(s):  
Mitsuhiro Wada ◽  
Mana Kuroki ◽  
Yuu Minami ◽  
Rie Ikeda ◽  
Yui Sekitani ◽  
...  
Keyword(s):  
Amino Acids ◽  
Fluorescence Detection ◽  
Dried Blood Spot ◽  
Newborn Baby ◽  
Sulfur Containing ◽  
Blood Spot
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