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1

Comparative study of performances of UHPLC-MS/MS and HPLC/UV methods for analysis of ziprasidone and its main impurities

Čarapić Marija, Marković Bojan, Pavlovic Milena, Agbaba Danica, Nikolic Katarina

Acta Chromatographica

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2023

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Vol. 35, no. 3

260--271

EN

Ziprasidone is the second generation antipsychotic drug with unique multipotent G-protein-coupled (GPCR) receptor binding profile. Since ziprasidone is a highly lipophilic and unstable compound, development of efficient method for a concurrent assay of ziprasidone and its main impurities was a very challenging task. The UHPLC-MS/MS method that we developed for simultaneous determination of ziprasidone and its main impurities (BITP, Chloroethyl-chloroindolinone, Zip-oxide, Zip-dimer, and Zip-BIT) was compared with some other related HPLC-UV methods of our own and other authorship. An increase of the mobile phase pH value from 2.5 to 4.7 units in the examined analytical methods influenced elution order of the investigated compounds. It was found out that the UHPLC-MS/MS method is more selective and sensitive than the earlier developed HPLC-UV method. Similar to our earlier HPLC-UV method, the UHPLC-MS/MS method is linear with a correlation coefficient (r) above 0.99 for all the analysed compounds, but with a negligibly lower precision and accuracy. Finally, with shorter analysis time, smaller column size and reduction of solvent consumption, UHPLC-MS/MS is assumed as a greener method than HPLC-UV for the ziprasidone purity assay. After transfer of the UHPLC-MS/MS method to the UHPLC-DAD system, suitability of the UHPLC-DAD method for routine control of ziprasidone and its main impurities is examined and confirmed based on the retained good selectivity, resolution and short analysis time.

2

High performance liquid chromatography coupled with mass spectrometry for simultaneous determination of rivastigmine and its metabolite in rat plasma

Sato Yuhki, Michihara Ayana, Nagatsuka Handa Yuka, Yamamoto Kouichi, Shirakawa Makoto, Katayama Hirokazu

Acta Chromatographica

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2022

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Vol. 34, no. 4

437--443

EN

Several studies on the pharmacokinetic parameters of antidementia drugs have reported that plasma concentration is linked to the drugs’ efficacy and adverse effects. At present, there is no quantitation method that is highly sensitive and can be applied to simultaneous monitoring of the pharmacokinetics of rivastigmine and its metabolites (NAP 226-90) in rat plasma. No methods fulfilling the assay validation requirements of the US Food and Drug Administration and the European Medicines Agency was also established. Therefore, this study developed a quantitative method for measuring rivastigmine and NAP 226-90 concentrations using high-performance liquid chromatography and tandem mass spectrometry, examining plasma samples after rivastigmine administration. Rat plasma samples were prepared via the protein precipitation method. The methods for measuring rivastigmine and NAP 226-90 concentrations showed good fit over wide ranges of 1–100 ng mL⁻¹ and 0.5–50 ng mL⁻¹, with lower limits of quantification at 1 ng mL⁻¹ and 0.5 ng mL⁻¹, respectively. The plasma concentrations of rivastigmine and NAP 226-90 in six healthy rats were successfully determined, demonstrating the feasibility of applying the developed method. Thus, this research has successfully developed a sensitive, selective method, to simultaneously quantify rivastigmine and NAP 226-90 concentrations in rat plasma and be applicable to a pharmacokinetic study.

3

Qualitative and quantitative analysis of seven signature components in the fruiting body of Antrodia cinnamomea by HPLC—ESI—MS/MS

Huang H. S., Hsu J. L., Yu C. C., Chang L. C., Chen C. R., Huang T. C., Chang C. J.

Acta Chromatographica

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2016

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Vol. 28, no. 3

387--402

EN

An accurate and rapid liquid chromatography–electrospray ionizaion– tandem mass spectrometry (LC—ESI—MS/MS) analytical method was developed and validated for the simultaneous determination of antcins A, B, C, H, and K, dehydroeburicoic acid, and 4,7-dimethoxy-5-methyl-1,3-benzodioxole in the extract and capsule of Antrodia cinnamomea (AC) fruiting body. These seven signature compounds were ionized using an electrospray ion source and analyzed by a triple-quadrupole mass analyzer under a multiple reaction monitoring (MRM) mode. The MRM transitions of m/z 453/409 (antcin A), m/z 467/408 (antcin B), m/z 469/425 (antcin C), m/z 485/413 (antcin H), m/z 487/407 (antcin K), m/z 467/337 (dehydroeburicoic acid), and m/z 197/139 (4,7-dimethoxy-5-methyl-1,3-benzodioxole) were used to quantify these seven components, respectively. Their calibration curves presented good linear regressions (R2 > 0.997) within the tested concentration range. The intra- and inter-day precisions were less than 1.97% and 2.53%, respectively. The overall recovery was in the range of 87.55%–95.41%. This validated high-performance liquid chromatography (HPLC)—MS/MS method offers promising applications for the accurate and rapid quantification of signature compounds in the fruiting body and its commercial products.

4

Determination of nicotine and three minor alkaloids in tobacco by hydrophilic interaction chromatography-tandem mass spectrometry

Taujenis L., Olšauskaitė V., Padarauskas A.

Acta Chromatographica

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2015

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Vol. 27, no. 2

373--385

EN

A reliable, sensitive and rapid method for determination of nicotine and three minor alkaloids (cotinine, anabasine and nornicotine) in tobacco by ultra-high performance liquid chromatography in hydrophilic interaction chromatography mode coupled with tandem mass spectrometry (HILIC-MS/MS) has been established. HILIC separation was performed on a BEH HILIC column using isocratic elution at 0.5 mL/min with acetonitrile:water (85:15, v/v) mobile phase containing 5 mmol/L ammonium acetate (pH 5.00). Separated analytes were determined by electrospray ionization MS/MS in the positive ion mode using multiple reaction monitoring. Alkaloids from tobacco were extracted in an ultrasonic bath for 10 min with acetonitrile:water mixture (8:2, v/v) containing 5 mmol/L ammonium acetate (pH 5.00). Limits of quantification were 10 μg/g for cotinine, 20 μg/g for anabasine and nornicotine, and 30 μg/g for nicotine. Mean recoveries from tobacco ranged between 94.8% and 104.1% for different analytes with relative standard deviations within 5%. The performance of the proposed method was tested for the extraction and determination of the four alkaloids in cigarette tobacco fillers, and satisfactory results were achieved.

5

Simultaneous determination of anthraquinone derivatives in Radix et Rhizoma Rhei-based medicines by ultra-performance LC-ESCI-MS/MS multiple reaction monitoring

Wang G. Y., Shi Y. P.

Acta Chromatographica

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2014

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Vol. 26, no. 2

229--242

EN

A new method using ultra-performance liquid chromatography (UPLC) in combination with tandem mass spectrometry and a multiple reaction monitoring mode (UPLC-MS/MS-MRM) was developed for simultaneous quantitative determination of anthraquinone derivatives in Radix et Rhizoma Rhei-based medicines. A multi-mode electrospray/chemical ionization (ESCI) and negative ion mode with [M-H]− and its fragments under collision-activated conditions were employed in MS/MS-MRM. The quantitative method was validated and applied to simultaneous determination of anthraquinone derivatives in 21 Radix et Rhizoma Rhei-based medicines. The limits of quantification were in the range of 3.90–9.09 ng mL -1. Average recoveries were between 95.5% and 99.8% with relative standard deviations from 1.8% to 5.3%.

6

Spektrometria mas – standard analityczny

Szewczyk R

LAB Laboratoria, Aparatura, Badania

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2013

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R. 18, nr 3

15--16

7

Identyfikacja diuretyków w moczu techniką ultrasprawnej chromatografii cieczowej połączonej z tandemową spektrometrią mas (UPLC/MS/MS)

Tszyrsznic W., Stańczyk D., Pokrywka A., Kwiatkowska D.

Wiadomości Chemiczne

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2010

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[Z] 64, 3-4

319-333

EN

Diuretics are medicines that intensify the diuresis process. There are several types of diuretics (high ceiling loop diuretics, thiazides, calcium-sparing diuretics, potassium-sparing diuretics, osmotic diuretics). Generally all of them increase excretion of water from a body. According to the Prohibited List published by the World Anti-Doping Agency diuretics make a group of substances which is prohibited in sport at all times (in- and out-of-competition). This review describes shortly an ultra performance liquid chromatography technique, chemical properties of diuretics named in the WADA Prohibited List as well as a developed analytical method with the use of UPLC/MS/MS technique for determination of diuretics and other doping agents (stimulants, masking agents) in urine samples in comparison with a GC/MS method used earlier. Detailed extraction procedure and comparison of application of several organic solvents during extraction process were given. Parameters of MS/MS method have also been given. The described method was validated in accordance with EURACHEM "The Fitness for Purpose of Analytical Methods: A Laboratory Guide to Method Validation and Related Topics". Limits of detection and recovery level for all compounds in the method were evaluated. The developed method allows to detect most of diuretics at the levels of 1/5 MRPL (Minimum Required Performance Limits) and fulfills all requirements of the World Anti-Doping Agency.

8

Determination of pesticides in selected cereal products by gas chromatography and ion trap mass spectrometry

Roszko M., Szymczyk K.

Chemia Analityczna

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2009

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Vol. 54, No. 6

1445-1464

EN

The aim of this study was to develop a simple and effective multi-residue screening method for determination of pesticides residues in cereal products. Ion trap-based mass spectrometer was used as a detector in a high-resolution chromatographic system. The method involved sample extraction with acetonitrile and cleanup of the extract on disposable SPE cartridges. Method performance was evaluated using some laboratory-made spiked samples. The obtained pesticides recoveries from the samples spiked at the level 0.01-0.4 mg kg-1 fell in the range 70-110% with relative standard deviation bellow 20% for most of the studied pesticides. The obtained limits of quantification for all investigated compounds were lower than or equal to 0.01 mg kg-1. The developed method has been practically used to determine 76 pesticides belonging to various chemical classes, which are most frequently analyzed in cereal products.

PL

Celem niniejszej pracy było opracowanie prostej i wydajnej przesiewowej metody chromatograficznego oznaczania pozostałości pestycydów w produktach zbożowych. Spektrometr mas w postaci pułapki jonowej wykorzystano jako detektor chromatograficzny. Metoda obejmowała ekstrakcję próbki za pomocą acetonitrylu i oczyszczanie ekstraktów z wykorzystaniem kolumienek SPE. Sprawność metody oszacowano na podstawie przygotowanych w laboratorium próbek fortyfikowanych. Wartości odzysku pestycydów z próbek fortyfi-kowanych na poziomie stężeń 0,01-0,4 mg kg-1 mieściły się w zakresie 70-110% przy wartości współczynnika zmienności poniżej 20% dla większości analizowanych substancji. Uzyskane wartości granicy oznaczania ilościowego wszystkich analizowanych substancji były równe lub niższe od 0.01 mg kg-1. Opracowaną metodę wykorzystano do oznaczania

9

Mass Spectrometric Decompositions of Platinum(II) Complexes with 1,3,4-Thiadiazoles and Dimethyl Sulfoxide. Changes in the Complexation Mode

Frański R., Gierczyk B.

Polish Journal of Chemistry

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2006

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Vol. 80, nr 3

453-462

EN

The platinum(II) complexes with 1,3,4-thiadiazoles and dimethyl sulfoxide have been studied by tandem mass spectrometry. Under the ion trap mass spectrometric condition, after the DMSO molecule(s) loss, changes have been observed in the complexation mode. They consisted in a fast conversion of one complex into another, provided that pyridine nitrogen atom contributes to the platinum cation complexation. The complexes studied have also shown a loss of the pyridine- or benzenenitrile molecule and HCl molecule. The eliminated HCl may contain a hydrogen atom originating from DMSO or from the aryl moiety. In the latter case, further decomposition of the ions formed involves (among others) a complex skeletal rearrangement yielding 2-thiopyridineplatinum cation.