Separation methods for tricyclic antiviral drugs

Suckow, Raymond F.

doi:10.1016/s0378-4347(01)00318-8

Cited by 20 publications

(9 citation statements)

References 44 publications

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“…Only the higher molecular weight derivative of tetramine, 4,10,13-trithia-1,3,5,7,9,11-hexaazatetracyclo[5.5.1.1 3,11 .1 5,9 ]pentadecane 4,10,13-tris(dioxide) ( Figure 1B), which forms in the presence of heat and acid, has been identified (22 ). Other adamantane compounds that are similar in structure to tetramine, including a class of antiviral drugs, retain full biological activity for decades when stored at room or refrigeration temperature (24 ).…”

Section: Evaluation Of Hypothesized Electrospray Ionization Mechanismmentioning

confidence: 99%

Quantitative Analysis of Tetramethylenedisulfotetramine (Tetramine) Spiked into Beverages by Liquid Chromatography−Tandem Mass Spectrometry with Validation by Gas Chromatography−Mass Spectrometry

Owens

Hok

Alcaraz

et al. 2009

J. Agric. Food Chem.

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Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD(50) = 0.1 mg/kg) used in hundreds of deliberate and accidental food poisoning events in China. This paper describes a method for the quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water, with cleanup by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography-mass spectrometry (GC-MS) operated in selected ion monitoring mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 μg/mL by LC-MS/MS versus 0.15 μg/mL for GC-MS. Fortifications of the beverages at 2.5 and 0.25 μg/mL were recovered ranging from 73 to 128% by liquid-liquid extraction for GC-MS analysis, from 13 to 96% by SPE, and from 10 to 101% by liquid-liquid extraction for LC-MS/MS analysis.

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Section: Evaluation Of Hypothesized Electrospray Ionization Mechanismmentioning

confidence: 99%

Quantitative Analysis of Tetramethylenedisulfotetramine (Tetramine) Spiked into Beverages by Liquid Chromatography−Tandem Mass Spectrometry with Validation by Gas Chromatography−Mass Spectrometry

Owens

Hok

Alcaraz

et al. 2009

J. Agric. Food Chem.

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“…The metabolic fate of rimantadine differs from other amantadinerelated drugs and only ca. 22% of the dose remained unmetabolized in urine [4,5].…”

Section: Introductionmentioning

confidence: 99%

Trace analysis of rimantadine in human urine after dispersive liquid liquid microextraction followed by liquid chromatography–post column derivatization

Zacharis

Tzanavaras

2019

J of Separation Science

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The first dispersive liquid liquid microextraction scheme followed by liquid chromatography-post column derivatization for the determination of the antiviral drug rimantadine in urine samples is demonstrated. The effect of the type and volume of organic extraction solvent, type and volume of disperser solvent, sample pH, ionic strength, extraction time, and centrifugation speed on the extraction efficiency were studied. Rimantadine and the internal standard (amantadine) were chromatographed using a reversed phase monolithic stationary phase with a mixture of equal volumes of methanol and phosphate buffer (pH = 3) as mobile phase. On-line postcolumn derivatization of the analyte was performed using a "two-stream" manifold with o-phthalaldehyde and N-acetyl-cysteine at alkaline medium. Under the optimized extraction conditions, the enrichment factor of rimantadine was 58. The linear range was 5-100 µg/L with correlation coefficient r of 0.9984 while the limit of detection achieved was 0.5 µg/L. The within-day and between-day precision for the tested concentration levels were less than 14.3% and the mean recoveries obtained from the spiked samples were ranged between 87.5 and 113.9%. The main advantages of the proposed method are the simplicity of operation, rapidity, low cost, and low limit of detection of the analyte. K E Y W O R D S rimantadine, dispersive liquid liquid microextraction, liquid chromatography, post-column derivatization, urine J Sep Sci 2020;43:631-638.2. The proposed DLLME scheme offers significant advantages including simplicity, low operation cost employing typical laboratory equipment, high extraction efficiency, and enrichment at a relative short extraction time.3. The sensitivity is almost 10-times higher compared to analogous methods using conventional SPE as sample treatment.4. Besides sensitivity, the combination of the DLLME with on-line PCD offers high selectivity, a feature that is always important in bioanalytical applications.

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“…The earlier works for the determination of RMT included analysis of RMT by GC -MS 2 , and using capillary zone electrophoresis 3 . New separation method for tricyclic antiviral drugs was developed 4 . Previous works included determination of RMT using IR Analysis 5 , online post column DRT 6 , fluorescent probe 7 , UV-visible spectrophotometry 8 , UHPLC coupled with orbitrap mass spectrometry 9 , use of AQSC for RMT analysis 10 , and simultaneous analysis using tandem mass spectrometry 11 .…”

Section: Introductionmentioning

confidence: 99%

"Development and Validation of a Rp-HPLC Method for the Analysis of Rimantadine Hydrochloride in Medicinal Form"

2018

RJC

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The aim of the research work was to conduct precolumn derivatization of Rimantadine hydrochloride (RMT) with Anthraquinone -2 -sulphonyl chloride (AQSC) to develop a validated, selective, precise and accurate RP-HPLC -UV method for the analysis of RMT -AQSC derivative in its Medicinal form. The isocratic mobile phase for the C -18 column consisted of Ethylnitrile and 0.005M 1 -octane sulfonic acid sodium salt monohydrate buffer (pH adjusted to 6.7) in 60:40 volume ratio. Flow rate maintained at one millilitre in one minute at ambient temperature. The ideal UV detection wavelength for RMT derivative was 259 nm. The retention time for both API and the medicine was 6.79 minutes. Linearity was satisfied over a range of 50 ppm to 250 ppm with a correlation coefficient (r) value 0.999. Percentage RSD for precision, accuracy and robustness were less than 2. The LOD and LOQ were 1.32 ppm and 4.0 ppm respectively. Validation was done as per 1CH guidelines and all the results were with in the limits.

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Separation methods for tricyclic antiviral drugs

Cited by 20 publications

References 44 publications

Quantitative Analysis of Tetramethylenedisulfotetramine (Tetramine) Spiked into Beverages by Liquid Chromatography−Tandem Mass Spectrometry with Validation by Gas Chromatography−Mass Spectrometry

Quantitative Analysis of Tetramethylenedisulfotetramine (Tetramine) Spiked into Beverages by Liquid Chromatography−Tandem Mass Spectrometry with Validation by Gas Chromatography−Mass Spectrometry

Trace analysis of rimantadine in human urine after dispersive liquid liquid microextraction followed by liquid chromatography–post column derivatization

"Development and Validation of a Rp-HPLC Method for the Analysis of Rimantadine Hydrochloride in Medicinal Form"

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