IDENTIFICATION AND QUANTIFICATION OF VERAPAMIL IN BLOOD AND URINE
Purpose: To adapt and validate an HPLC method for verapamil determination in blood and urine samples. Materials/Methods: Identification of verapamil and its metabolites was made by means of gas-chromatography, using Agilent 7890B/5977A GC-MS system featuring a DB-1701 column. Quantification was don...
| Main Authors: | , , , |
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| Format: | Article |
| Language: | English |
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Peytchinski Publishing
2020-10-01
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| Series: | Journal of IMAB |
| Subjects: | |
| Online Access: | https://www.journal-imab-bg.org/issues-2020/issue4/2020vol26-issue4-3403-3407.pdf |
| _version_ | 1819172371992412160 |
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| author | Georgi Bonchev Snezha Zlateva Petko Marinov Ivelina Stefanova |
| author_facet | Georgi Bonchev Snezha Zlateva Petko Marinov Ivelina Stefanova |
| author_sort | Georgi Bonchev |
| collection | DOAJ |
| description | Purpose: To adapt and validate an HPLC method for verapamil determination in blood and urine samples.
Materials/Methods: Identification of verapamil and its metabolites was made by means of gas-chromatography, using Agilent 7890B/5977A GC-MS system featuring a DB-1701 column. Quantification was done by means of liquid chromatography on Agilent 1260 series HPLC, equipped with Zorbax Extend-C18 column and both diode-array and fluorescent detection modules. Blood and urine specimens were taken from patients of the Clinic for intensive treatment of acute intoxications and toxicoallergies within the course of their treatment.
Results: GC-MS identification of verapamil and its metabolites was carried out after simple liquid-liquid extraction of samples without further chemical derivatization. Adapted HPLC method for quantification require isocratic conditions and mobile phase, consisted of phosphate buffer (pH 2.7; 10 mM) containing 1.5 ml L–1 triethylamine – acetonitrile (70:30, v/v) at 20oC, flow-rate 1.0 mL/min and FLD detection (excitation: 203 nm, emission: 320 nm). The method was demonstrated to be linear within the whole region of interest (4.6-4600 ng mL–1) with excellent accuracy (101.7-102.2%) and inter-day precision (5.81%) as well as good analytical recovery (81.2%) and LOQ (7.0 ng mL–1).
Conclusion: A precise and easy to use method for verapamil detection and quantification is developed. The method is applicable as a routine procedure in the Laboratory of analytical toxicology for both diagnosis clarification in cases of acute intoxications and therapeutic drug monitoring. |
| first_indexed | 2024-12-22T20:06:08Z |
| format | Article |
| id | doaj.art-cb8a1ce9478a4223abf5cd4a3d5b0589 |
| institution | Directory Open Access Journal |
| issn | 1312-773X |
| language | English |
| last_indexed | 2024-12-22T20:06:08Z |
| publishDate | 2020-10-01 |
| publisher | Peytchinski Publishing |
| record_format | Article |
| series | Journal of IMAB |
| spelling | doaj.art-cb8a1ce9478a4223abf5cd4a3d5b05892022-12-21T18:14:07ZengPeytchinski PublishingJournal of IMAB1312-773X2020-10-012643403340710.5272/jimab.2020264.3403IDENTIFICATION AND QUANTIFICATION OF VERAPAMIL IN BLOOD AND URINEGeorgi Bonchev0https://orcid.org/0000-0002-6220-4020Snezha Zlateva1Petko Marinov2Ivelina Stefanova3Clinic for Intensive Treatment of Acute Intoxications and Toxicoallergies, Naval Hospital – Varna, Military Medical Academy, BulgariaClinic for Intensive Treatment of Acute Intoxications and Toxicoallergies, Naval Hospital – Varna, Military Medical Academy, BulgariaClinic for Intensive Treatment of Acute Intoxications and Toxicoallergies, Naval Hospital – Varna, Military Medical Academy, BulgariaClinic for Intensive Treatment of Acute Intoxications and Toxicoallergies, Naval Hospital – Varna, Military Medical Academy, BulgariaPurpose: To adapt and validate an HPLC method for verapamil determination in blood and urine samples. Materials/Methods: Identification of verapamil and its metabolites was made by means of gas-chromatography, using Agilent 7890B/5977A GC-MS system featuring a DB-1701 column. Quantification was done by means of liquid chromatography on Agilent 1260 series HPLC, equipped with Zorbax Extend-C18 column and both diode-array and fluorescent detection modules. Blood and urine specimens were taken from patients of the Clinic for intensive treatment of acute intoxications and toxicoallergies within the course of their treatment. Results: GC-MS identification of verapamil and its metabolites was carried out after simple liquid-liquid extraction of samples without further chemical derivatization. Adapted HPLC method for quantification require isocratic conditions and mobile phase, consisted of phosphate buffer (pH 2.7; 10 mM) containing 1.5 ml L–1 triethylamine – acetonitrile (70:30, v/v) at 20oC, flow-rate 1.0 mL/min and FLD detection (excitation: 203 nm, emission: 320 nm). The method was demonstrated to be linear within the whole region of interest (4.6-4600 ng mL–1) with excellent accuracy (101.7-102.2%) and inter-day precision (5.81%) as well as good analytical recovery (81.2%) and LOQ (7.0 ng mL–1). Conclusion: A precise and easy to use method for verapamil detection and quantification is developed. The method is applicable as a routine procedure in the Laboratory of analytical toxicology for both diagnosis clarification in cases of acute intoxications and therapeutic drug monitoring.https://www.journal-imab-bg.org/issues-2020/issue4/2020vol26-issue4-3403-3407.pdfverapamilgc-mshplcacute intoxicationstherapeutic drug monitoring |
| spellingShingle | Georgi Bonchev Snezha Zlateva Petko Marinov Ivelina Stefanova IDENTIFICATION AND QUANTIFICATION OF VERAPAMIL IN BLOOD AND URINE Journal of IMAB verapamil gc-ms hplc acute intoxications therapeutic drug monitoring |
| title | IDENTIFICATION AND QUANTIFICATION OF VERAPAMIL IN BLOOD AND URINE |
| title_full | IDENTIFICATION AND QUANTIFICATION OF VERAPAMIL IN BLOOD AND URINE |
| title_fullStr | IDENTIFICATION AND QUANTIFICATION OF VERAPAMIL IN BLOOD AND URINE |
| title_full_unstemmed | IDENTIFICATION AND QUANTIFICATION OF VERAPAMIL IN BLOOD AND URINE |
| title_short | IDENTIFICATION AND QUANTIFICATION OF VERAPAMIL IN BLOOD AND URINE |
| title_sort | identification and quantification of verapamil in blood and urine |
| topic | verapamil gc-ms hplc acute intoxications therapeutic drug monitoring |
| url | https://www.journal-imab-bg.org/issues-2020/issue4/2020vol26-issue4-3403-3407.pdf |
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