Method development and validation for rapid quantification of hydroxychloroquine in human blood using liquid chromatography-tandem mass spectrometry
Identifieur interne : 000055 ( PascalFrancis/Curation ); précédent : 000054; suivant : 000056Method development and validation for rapid quantification of hydroxychloroquine in human blood using liquid chromatography-tandem mass spectrometry
Auteurs : Ling-Zhi Wang [Singapour] ; Rina Yue-Ling Ong [Singapour] ; Tan-Min Chin [Singapour] ; Win-Lwin Thuya [Singapour] ; Seow-Ching Wan [Singapour] ; Andrea Li-Ann Wong [Singapour] ; Sui-Yung Chan [Singapour] ; Paul C. Ho [Singapour] ; Boon-Cher Goh [Singapour]Source :
- Journal of pharmaceutical and biomedical analysis [ 0731-7085 ] ; 2012.
Descripteurs français
- Pascal (Inist)
- Wicri :
- topic : Analyse quantitative, Homme.
English descriptors
- KwdEn :
Abstract
A novel and specific liquid chromatography-tandem mass spectrometric method (LC-MS/MS) was developed and validated for the quantification of hydroxychloroquine in human blood using its stable labeled isotope, hydroxychloroquine-d4 as the internal standard. Chromatographic separation of analytes was achieved using an Agilent ZORBAX Eclipse XDB - C8 analytical HPLC column (50 mm x 2.1 mm, 5 μm). The mobile phase comprising water containing 0.1% formic acid-acetonitrile (94:6, v/v) was delivered isocratically at a flow rate of 0.5 mL/min. The column effluent was detected by API 4000 triple quadrupole mass spectrometer using electrospray ionization (ESI) and monitored by multiple reaction monitoring with positive mode. The precursor to product ion transitions of m/z 336 → 247 and m/z 340 → 251 were used to measure the analyte and IS, respectively. The assay demonstrated a good linear dynamic range of 5-2000 ng/mL for hydroxychloroquine in human blood, with coefficient of determination (r2) of =0.9999. The values for intra-day and inter-day precisions of hydroxychloroquine were ≤7.86% with the accuracies ranged from 93.8% to 107.6%. The chromatographic run time was 3 min, making it possible to achieve a high throughput analysis. This method was used as a bio-analytical tool in a phase 1 clinical trial to quantify blood hydroxychloroquine concentrations in patients with non-small cell lung cancer receiving both hydroxychloroquine and gefitinib in their treatment.
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<front><div type="abstract" xml:lang="en">A novel and specific liquid chromatography-tandem mass spectrometric method (LC-MS/MS) was developed and validated for the quantification of hydroxychloroquine in human blood using its stable labeled isotope, hydroxychloroquine-d4 as the internal standard. Chromatographic separation of analytes was achieved using an Agilent ZORBAX Eclipse XDB - C8 analytical HPLC column (50 mm x 2.1 mm, 5 μm). The mobile phase comprising water containing 0.1% formic acid-acetonitrile (94:6, v/v) was delivered isocratically at a flow rate of 0.5 mL/min. The column effluent was detected by API 4000 triple quadrupole mass spectrometer using electrospray ionization (ESI) and monitored by multiple reaction monitoring with positive mode. The precursor to product ion transitions of m/z 336 → 247 and m/z 340 → 251 were used to measure the analyte and IS, respectively. The assay demonstrated a good linear dynamic range of 5-2000 ng/mL for hydroxychloroquine in human blood, with coefficient of determination (r<sup>2</sup>
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</fC03>
<fC03 i1="05" i2="X" l="SPA"><s0>Hombre</s0>
<s5>05</s5>
</fC03>
<fC03 i1="06" i2="X" l="FRE"><s0>Liquide biologique</s0>
<s5>06</s5>
</fC03>
<fC03 i1="06" i2="X" l="ENG"><s0>Biological fluid</s0>
<s5>06</s5>
</fC03>
<fC03 i1="06" i2="X" l="SPA"><s0>Líquido biológico</s0>
<s5>06</s5>
</fC03>
<fC03 i1="07" i2="X" l="FRE"><s0>Sang</s0>
<s5>07</s5>
</fC03>
<fC03 i1="07" i2="X" l="ENG"><s0>Blood</s0>
<s5>07</s5>
</fC03>
<fC03 i1="07" i2="X" l="SPA"><s0>Sangre</s0>
<s5>07</s5>
</fC03>
<fC03 i1="08" i2="X" l="FRE"><s0>Chromatographie HPLC</s0>
<s5>08</s5>
</fC03>
<fC03 i1="08" i2="X" l="ENG"><s0>HPLC chromatography</s0>
<s5>08</s5>
</fC03>
<fC03 i1="08" i2="X" l="SPA"><s0>Cromatografía HPLC</s0>
<s5>08</s5>
</fC03>
<fC03 i1="09" i2="X" l="FRE"><s0>Spectrométrie masse tandem</s0>
<s5>09</s5>
</fC03>
<fC03 i1="09" i2="X" l="ENG"><s0>Mass spectrometry MS/MS</s0>
<s5>09</s5>
</fC03>
<fC03 i1="09" i2="X" l="SPA"><s0>Espectrometría masa en tándem</s0>
<s5>09</s5>
</fC03>
<fC03 i1="10" i2="X" l="FRE"><s0>Antiparasitaire</s0>
<s5>23</s5>
</fC03>
<fC03 i1="10" i2="X" l="ENG"><s0>Parasiticide</s0>
<s5>23</s5>
</fC03>
<fC03 i1="10" i2="X" l="SPA"><s0>Antiparasitario</s0>
<s5>23</s5>
</fC03>
<fC03 i1="11" i2="X" l="FRE"><s0>Antipaludique</s0>
<s5>24</s5>
</fC03>
<fC03 i1="11" i2="X" l="ENG"><s0>Antimalarial</s0>
<s5>24</s5>
</fC03>
<fC03 i1="11" i2="X" l="SPA"><s0>Antipalúdico</s0>
<s5>24</s5>
</fC03>
<fC03 i1="12" i2="X" l="FRE"><s0>Antirhumatismal</s0>
<s5>25</s5>
</fC03>
<fC03 i1="12" i2="X" l="ENG"><s0>Antirheumatic agent</s0>
<s5>25</s5>
</fC03>
<fC03 i1="12" i2="X" l="SPA"><s0>Antireumático</s0>
<s5>25</s5>
</fC03>
<fC03 i1="13" i2="X" l="FRE"><s0>LC MS MS</s0>
<s4>INC</s4>
<s5>86</s5>
</fC03>
<fN21><s1>114</s1>
</fN21>
<fN44 i1="01"><s1>OTO</s1>
</fN44>
<fN82><s1>OTO</s1>
</fN82>
</pA>
</standard>
</inist>
</record>
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