Indacaterol determination in human urine : validation of a liquid-liquid extraction and liquid chromatography-tandem mass spectrometry analytical method
BACKGROUND: Indacaterol is a novel once-a-day inhaled ultra-long-acting β2-agonist. Quantitative bioanalysis supports pharmacokinetic and clinical research. The aim of the current work was to validate an in-house developed high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) analytical method for indacaterol determination in human urine samples.
METHODS: A liquid-liquid extraction method has been developed to extract indacaterol from human urine samples using ethyl acetate. Indacaterol dry extract was reconstituted with 200 μL of the mobile phase (acidified water:methanol (30:70, v/v)) of which 5 μL was needed for the HPLC-MS/MS analysis. Indacaterol was eluted on a reversed C18 stationary phase with an isocratic mobile phase at a flow of 1 mL/min. Formoterol was the internal standard (IS). The MS/MS detection was employed with a turbo-ion spray ionization in the positive ion mode. A consensus of the international Guidelines for Bioanalytical Method Validation was followed.
RESULTS: Indacaterol was detected at a mass to charge ratio (m/z) of 393.3 and its MS/MS daughter at 173.2. The retention times of indacaterol and IS were 1.60 and 1.20 min, respectively. Validated calibration curves were linear over a range of 0.075-100 ng/mL with correlation coefficients (r)≥0.990. The curves' regression weighting factor was 1/x. Method specificity was established in six different human urine batches. No matrix interference was observed. The intra- and inter-batch precision and accuracy within±20% (at lower limit) and±15% (other quality control (QC) levels) were confirmed. The indacaterol mean recovery (precision) percentages at Low, Mid, and High QC levels were 93.5 (3.84), 89.8 (2.15), and 92.2 (2.17), respectively. Short-term, long-term, freeze-thaw, and auto-sampler stability results were accepted.
CONCLUSIONS: A specific, accurate and precise HPLC-MS/MS method has been validated for indacaterol quantification in human urine. This simple method is reproducible and robust to support future, indacaterol-related pharmacokinetic, bioequivalence and clinical studies.
| Medienart: |
E-Artikel |
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| Erscheinungsjahr: |
2015 |
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| Erschienen: |
2015 |
| Enthalten in: |
Zur Gesamtaufnahme - volume:28 |
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| Enthalten in: |
Journal of aerosol medicine and pulmonary drug delivery - 28(2015), 3 vom: 17. Juni, Seite 202-10 |
| Sprache: |
Englisch |
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| Beteiligte Personen: |
Ammari, Wesam G [VerfasserIn] |
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| Links: |
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| Anmerkungen: |
Date Completed 18.03.2016 Date Revised 10.12.2019 published: Print-Electronic Citation Status MEDLINE |
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| doi: |
10.1089/jamp.2014.1153 |
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| funding: |
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| Förderinstitution / Projekttitel: |
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| PPN (Katalog-ID): |
NLM241978904 |
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| 100 | 1 | |a Ammari, Wesam G |e verfasserin |4 aut | |
| 245 | 1 | 0 | |a Indacaterol determination in human urine |b validation of a liquid-liquid extraction and liquid chromatography-tandem mass spectrometry analytical method |
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| 500 | |a Date Completed 18.03.2016 | ||
| 500 | |a Date Revised 10.12.2019 | ||
| 500 | |a published: Print-Electronic | ||
| 500 | |a Citation Status MEDLINE | ||
| 520 | |a BACKGROUND: Indacaterol is a novel once-a-day inhaled ultra-long-acting β2-agonist. Quantitative bioanalysis supports pharmacokinetic and clinical research. The aim of the current work was to validate an in-house developed high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) analytical method for indacaterol determination in human urine samples | ||
| 520 | |a METHODS: A liquid-liquid extraction method has been developed to extract indacaterol from human urine samples using ethyl acetate. Indacaterol dry extract was reconstituted with 200 μL of the mobile phase (acidified water:methanol (30:70, v/v)) of which 5 μL was needed for the HPLC-MS/MS analysis. Indacaterol was eluted on a reversed C18 stationary phase with an isocratic mobile phase at a flow of 1 mL/min. Formoterol was the internal standard (IS). The MS/MS detection was employed with a turbo-ion spray ionization in the positive ion mode. A consensus of the international Guidelines for Bioanalytical Method Validation was followed | ||
| 520 | |a RESULTS: Indacaterol was detected at a mass to charge ratio (m/z) of 393.3 and its MS/MS daughter at 173.2. The retention times of indacaterol and IS were 1.60 and 1.20 min, respectively. Validated calibration curves were linear over a range of 0.075-100 ng/mL with correlation coefficients (r)≥0.990. The curves' regression weighting factor was 1/x. Method specificity was established in six different human urine batches. No matrix interference was observed. The intra- and inter-batch precision and accuracy within±20% (at lower limit) and±15% (other quality control (QC) levels) were confirmed. The indacaterol mean recovery (precision) percentages at Low, Mid, and High QC levels were 93.5 (3.84), 89.8 (2.15), and 92.2 (2.17), respectively. Short-term, long-term, freeze-thaw, and auto-sampler stability results were accepted | ||
| 520 | |a CONCLUSIONS: A specific, accurate and precise HPLC-MS/MS method has been validated for indacaterol quantification in human urine. This simple method is reproducible and robust to support future, indacaterol-related pharmacokinetic, bioequivalence and clinical studies | ||
| 650 | 4 | |a Journal Article | |
| 650 | 4 | |a Research Support, Non-U.S. Gov't | |
| 650 | 4 | |a Validation Study | |
| 650 | 4 | |a LC-MS/MS method | |
| 650 | 4 | |a bioanalytical method | |
| 650 | 4 | |a indacaterol | |
| 650 | 4 | |a liquid-liquid extraction | |
| 650 | 4 | |a urine | |
| 650 | 4 | |a validation | |
| 650 | 7 | |a Adrenergic beta-2 Receptor Agonists |2 NLM | |
| 650 | 7 | |a Indans |2 NLM | |
| 650 | 7 | |a Quinolones |2 NLM | |
| 650 | 7 | |a indacaterol |2 NLM | |
| 650 | 7 | |a 8OR09251MQ |2 NLM | |
| 700 | 1 | |a Al-Qadhi, Zainab |e verfasserin |4 aut | |
| 700 | 1 | |a Khalil, Mohammad |e verfasserin |4 aut | |
| 700 | 1 | |a Tayyem, Rabab |e verfasserin |4 aut | |
| 700 | 1 | |a Qammaz, Samir |e verfasserin |4 aut | |
| 700 | 1 | |a Oriquat, Ghaleb |e verfasserin |4 aut | |
| 700 | 1 | |a Basheti, Iman A |e verfasserin |4 aut | |
| 700 | 1 | |a Chrystyn, Henry |e verfasserin |4 aut | |
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