scholarly journals Determination of oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin in mouse blood by UPLC-MS/MS and its application to pharmacokinetics

2021 ◽  
Author(s):  
Zheng Yu ◽  
Fan Chen ◽  
Yinan Jin ◽  
Minyue Zhou ◽  
Xianqin Wang ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Oroxylin A ◽  
Mouse Blood ◽  
Multiple Reactions ◽  
Caudal Vein ◽  
The Matrix ◽  
Positive Ion

Abstract In this study, a UPLC-MS/MS method was developed to measure the concentrations of the flavonoids oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin in the blank mouse blood, and the method was then used in the measurement of the pharmacokinetics of the compounds in mice. Oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin were administered intravenously at a dose of 5 mg kg−1, and the mouse blood (20 μL) was withdrawn from the caudal vein 0.08333, 0.25, 0.5, 1, 2, 4, 6, 8, and 10 h after administration. The mobile phase used for chromatographic separation by gradient elution was composed of acetonitrile and water (0.1% formic acid). The analytes were detected by operating in electrospray ionization (ESI) positive-ion mode using multiple reactions monitoring (MRM). The intra-day and inter-day accuracy ranged from 86.2 to 109.3%, the intra-day precision was less than 14%, and the inter-day precision was less than 15%. The matrix effect ranged from 85.3 to 111.3%, and the recovery of the analytes after protein precipitation were all above 78.2%. This method had the advantages of high sensitivity, accuracy, and recovery, and it had excellent selectivity, which enabled it to be applied to measuring the pharmacokinetics of the analytes in mice.

scholarly journals Simultaneous Determination of Six Uncaria Alkaloids in Mouse Blood by UPLC–MS/MS and Its Application in Pharmacokinetics and Bioavailability

2020 ◽  
Vol 2020 ◽  
pp. 1-11
Author(s):  
Lianguo Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Meiling Zhang
Keyword(s):  
Simultaneous Determination ◽  
Oral Absorption ◽  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Mouse Blood ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

A specific ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed for the simultaneous determination of six Uncaria alkaloids in mouse blood with midazolam as the internal standard (IS). Only 20 μL blood was needed for sample preparation, and the protein was precipitated with acetonitrile. The UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm) was used for chromatographic separation. The mobile phase consisted of 0.1% formic acid and acetonitrile with gradient elution within 5.5 min. Multiple reaction monitoring (MRM) and the positive electrospray ionization model were used for quantitative analysis. The accuracy of the UPLC-MS/MS method ranged from 86.5% to 110.4%. The precision for intraday and interday was ≤15% each. The mean recovery and the matrix effects were found to be 64.4-86.8% and 94.1-109.4%, respectively. The calibration curves in blood were linear in the range of 1-1000 ng/mL with a favorable correlation coefficient (r2) of 0.995. The pharmacokinetic results showed that six Uncaria alkaloids metabolized rapidly in mice with a half-life between 0.6 h and 4.4 h. The bioavailability of corynoxeine, isocorynoxeine, rhynchophylline, isorhynchophylline, hirsutine, and hirsuteine was 27.3%, 32.7%, 49.4%, 29.5%, 68.9%, and 51.0%, respectively, which showed satisfactory oral absorption of each alkaloid.

scholarly journals Determination of narciclasine in mouse blood by UPLC-MS/MS and its application to a pharmacokinetic study

2021 ◽  
Author(s):  
Ke Ren ◽  
Tiantian Feng ◽  
Hai Shi ◽  
Jianshe Ma ◽  
Yongxi Jin
Keyword(s):  
Intravenous Administration ◽  
Pharmacokinetic Study ◽  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Hydroxy Derivative ◽  
Reaction Monitoring ◽  
Mouse Blood ◽  
The Matrix

AbstractNarciclasine is a 7-hydroxy derivative of lycorisidine. It was the first alkaloid isolated from the stem of narcissus (Amaryllidaceae) in 1967. Six mice were given narciclasine (5 mg/kg) by intravenous administration. A UPLC-MS/MS method was developed to determine narciclasine in mouse blood. Tectorigenin (internal standard, IS) and narciclasine were gradient eluted by mobile phase of methanol and 0.1% formic acid in a BEH C18 column. The multiple reaction monitoring (MRM) of m/z 308.1→248.1 for narciclasine and m/z 301.1→286.0 for IS with an electrospray ionization (ESI) source was used for quantitative determination. The calibration curve ranged from 1 to 6,000 ng/mL. The accuracy was from 92.5 to 107.3%, and the matrix effect was between 103.6 and 107.4%. The developed UPLC-MS/MS method was successfully applicated to a pharmacokinetic study of narciclasine in mice after intravenous administration (5 mg/kg).

scholarly journals Pharmacokinetics of tectorigenin, tectoridi, irigenin, and iridin in mouse blood after intravenous administration by UPLC-MS/MS

2021 ◽  
Author(s):  
Jianbo Li ◽  
Yuqi Yao ◽  
Minyue Zhou ◽  
Zheng Yu ◽  
Yinan Jin ◽  
...  
Keyword(s):  
Intravenous Administration ◽  
Detection Method ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Reaction Monitoring ◽  
Mouse Blood ◽  
Target Analytes ◽  
The Matrix ◽  
Positive Ion

AbstractTectorigenin, tectoridin, irigenin, and iridin are the four most predominant compounds present in She Gan. She Gan has been used in traditional Chinese medicine because of its anti-inflammatory, hepatoprotective, anti-tumor, antioxidant, phytoestrogen-like properties. In this paper, a UPLC-MS/MS method was developed to measure the pharmacokinetics of tectorigenin, tectoridin, irigenin, iridin after intravenous administration in mice. A UPLC BEH C18 (50 mm × 2.1 mm, 1.7 μm particle size) chromatographic column was utilized for separation of the four target analytes and internal standard (IS), and the analysis of blood plasma samples; the mobile phase consisted of an acetonitrile-water (w/0.1% formic acid) gradient elution. Electron spray ionization (ESI) positive-ion mode and multiple reaction monitoring (MRM) mode was used for quantitative analysis of the analytes and internal standard. The four compounds were administered intravenously (sublingual) at doses of 5 mg/kg. After blood sampling, samples were processed and then analyzed by UPLC-MS/MS. The linearity of the method was robust over the concentration range of 2–5,000 ng/mL. The intra-day precision of the analysis was within 15%, the inter-day precision was within 12%, and the accuracy was between 92% and 110%. The recoveries were 65–68%, and the matrix effect was 93–109%. The established UPLC-MS/MS detection method was then successfully applied to study the pharmacokinetics of tectorigenin, tectoridin, irigenin, iridin in mice.

Simultaneous Determination of Alogliptin, Linagliptin, Saxagliptin, and Sitagliptin in Bulk Drug and Formulation by UPLC Q-TOF-MS

2020 ◽  
Vol 17 (1) ◽  
pp. 95-105
Author(s):  
Ramji Rathod ◽  
Faraat Ali ◽  
Amrish Chandra ◽  
Robin Kumar ◽  
Meenakshi Dahiya ◽  
...  
Keyword(s):  
Internal Standard ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Pharmaceutical Dosage Forms ◽  
Sensitivity And Selectivity ◽  
The Mean ◽  
Bulk Drug ◽  
Positive Ion ◽  
Higher Sensitivity

Background: A simple and sensitive Ultra Performance Liquid Chromatography-Mass Spectrometry method was developed and validated to measure the concentrations of Alogliptin (ALO), Linagliptin (LIN), Saxagliptin (SAX), and Sitagliptin (SIT) using Pioglitazone (PIO) as an internal standard. Methods: Chromatographic separation of six gliptins was achieved on a C-18 column (100×2.1 mm, 2.7 μm) using a mobile phase consisting of formic acid in water, 0.1%v/v: acetonitrile in gradient elution. Electrospray ionization (ESI) source was operated in the positive ion mode. Targeted MS/MS mode on a QTOF MS was used to quantify the drug utilizing the transitions of 340.1(m/z), 473.2 (m/z), 316.2 (m/z), 408.1 (m/z), and 357.1 (m/z) for ALO, LIN, SAX, SIT and PIO respectively. Results: As per ICH Q2R1 guidelines, a detailed validation of the method was carried out and the standard curves were found to be linear over the concentration ranges of 1516.0-4548.1 ng mL-1, 519.8- 1559.4 ng mL-1, 1531.4-4594.3 ng mL-1and 1519.6-4558.8 ng mL-1 for ALO, LIN, SAX and SIT respectively. Precision and accuracy results were within the acceptable limits. The mean recovery was found to be 98.8 _ 0.76 % (GEM), 102.2 _ 1.59 % (LIN), 95.3 _ 2.74 % (SAX) and 99.2 _ 1.75 % (SIT) respectively. Conclusions: The optimized validated UPLC QTOF-MS/MS method offered the advantage of shorter analytical times and higher sensitivity and selectivity. The optimized method is suitable for application in quantitative analysis of pharmaceutical dosage forms for QC laboratory.

Development and Validation of HPLC Determination of related Substances in A Novel Anticonvulsant agent Epimidin

2021 ◽  
pp. 3223-3231
Author(s):  
Hanna I. Severina ◽  
Svitlana M. Gubar ◽  
Ivan V. Bezruk ◽  
Anna S. Materiienko ◽  
Liudas Ivanauskas ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Phosphate Buffer Solution ◽  
Anticonvulsant Drug ◽  
Strong Acid ◽  
Gradient Elution ◽  
Stress Conditions ◽  
Drug Candidate ◽  
Buffer Solution ◽  
Related Substances

1-(4-methoxyphenyl)-5-[2-[4-(4-methoxyphenyl)piperazin-1-yl]-2-oxo-ethyl]pyrazolo[3,4-d]pyrimidin-4-one has been reported as a promising new anticonvulsant drug candidate with a code name “Epimidin”. A new HPLC method for the related substances determination of potential active pharmaceutical ingredient has been developed and validated. The method uses ACE C18 column (250x4.6mm, 5µm) and gradient elution. Mobile phase consisted of a mixture of methanol R (mobile phase A) and phosphate buffer solution with triethanolamine, adjusted to pH 7.0 (mobile phase B). During the analysis, the ratio of mobile phases was changing according to a gradient mode at a flow rate of 1ml/min. The DAD detection was set at 240nm. The method was validated according to the ICH guidelines and requirements of State Pharmacopoeia of Ukraine. Drug substance was thoroughly explored for stability assessments under various stress conditions such as high temperature, as well as the influence of strong acid and base and oxidizing agents. The obtained solutions were analyzed by HPLC and LC/MS. It has been shown that the substance Epimidin was not resistant to the action of peroxide, alkali and acid decomposition – the mentioned stress conditions lead to the formation of unidentified impurities.

scholarly journals Determination of Nitroimidazole Residues in Porcine Urine by Liquid Chromatography/TandemMass Spectrometry

2006 ◽  
Vol 89 (4) ◽  
pp. 1116-1119 ◽  
Author(s):  
Xi Xia ◽  
Xiaowei Li ◽  
Jianzhong Shen ◽  
Suxia Zhang ◽  
Shuangyang Ding ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Solid Phase ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Mass Spectrometry System ◽  
Ionization Mode ◽  
Positive Ion ◽  
Mode A

Abstract A reliable and sensitive method was developed for determination of nitroimidazoles in porcine urine. Sample preparation involves an extraction with ethyl acetate, followed by a solid-phase extraction cleanup step. The final extract is injected into the liquid chromatography/tandem mass spectrometry system in the positive-ion electrospray ionization mode. A C8 column with water and acetonitrile as the mobile phase is used for chromatographic separation under gradient conditions. Overall average recoveries ranged from 83 to 107%. The limits of detection ranged from 0.03 to 0.05 ng/mL, and the limits of quantitation, from 0.1 to 0.2 ng/mL.

scholarly journals Simultaneous Determination of Eight Synthetic Permitted and Five Commonly Encountered Nonpermitted Food Colors in Various Food Matrixes by High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (5) ◽  
pp. 1503-1514 ◽  
Author(s):  
Sumita Dixit ◽  
Subhash K Khanna ◽  
Mukul Das
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Food Category ◽  
Food Commodities ◽  
Food Colors

Abstract A simple and sensitive HPLC method has been developed for the simultaneous determination of eight permitted food colors and five commonly encountered nonpermitted colors in various food commodities, including sugar-, fat-, and starch-based food matrixes. The method uses a specific food category-based cleanup/treatment procedure before color extraction to avoid the interference of food matrixes, and to obtain the optimal color extraction. Analysis was performed on a reversed-phase C18 -Bondapak column with ammonium acetate and acetonitrile gradient elution as the mobile phase; a programmable max-specific visible detection was used to monitor colors to obtain the higher sensitivity and expanded scope needed for multicolor blends having diverse absorption maxima. All colors showed good linearity, with regression coefficients of 0.99740.9999. The LOD and LOQ values ranged from 0.01 to 0.12 mg/L, and from 0.04 to 0.83 mg/L or mg/kg, respectively. The intraday and interday precision tests produced good RSD values, and the recoveries from different food matrixes ranged from 82 to 104%. The method offers high sensitivity for analysis of a wide variety of food matrixes containing a broad scope of multicolor blends. Two nonpermitted colors, orange II and metanil yellow, were found. Also, a number of samples contained permitted colors at levels two-to seven-fold higher than those prescribed.

scholarly journals Simultaneous Determination of Rimsulfuron and Haloxyfop-P-methyl and Its Metabolite Haloxyfop in Tobacco Leaf by LC-MS/MS

2019 ◽  
Vol 102 (5) ◽  
pp. 1632-1640
Author(s):  
Yurong Yu ◽  
Shan Zhao ◽  
Ya Yang ◽  
Ya Chen ◽  
Daimei Qiu ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Weed Management ◽  
Matrix Effects ◽  
High Sensitivity ◽  
Tobacco Leaf ◽  
Extraction Solvent ◽  
Nicotiana Tabacum L ◽  
The Matrix ◽  
Pretreatment Conditions

Abstract Background: Tobacco (Nicotiana tabacum L.), is an important economic crop. In China, the use of rimsulfuron and haloxyfop-P-methyl herbicides for weed management during the planting period is necessary to improve the production of tobacco. Objective: To establish and validate a quick, easy, cheap, effective, rugged, and safe LC-MS/MS method to determine rimsulfuron, haloxyfop-P-methyl, and haloxyfop in tobacco leaf samples. Methods: We optimized MS/MS conditions and chromatographic conditions for optimal detection conditions. The extraction solvent and sorbent were optimized, and the analysis of variance was applied to analyze the pretreatment method to obtain the optimal pretreatment conditions. Results: The validation results showed that the proposed method exhibited good linearity (R2 > 0.9978), satisfactory recovery (72.51–101.60%) and low LOQ (0.02–1.00 mg/kg). The matrix effects of the three analytes in the two tobacco leaf matrixes were different. The dissipation results showed that the half-lives of rimsulfuron and haloxyfop-P-methyl in fresh tobacco leaf samples were ranged from 2.4 to 3.7 days. The final residues of rimsulfuron, haloxyfop-P-methyl, and haloxyfop in flue-cured tobacco leaf samples were all lower than the LOQ. Conclusions: The results demonstrate that the developed method could be used to detect rimsulfuron, haloxyfop-P-methyl, and haloxyfop in tobacco leaf matrixes. Highlights: A method for simultaneous determination of rimsulfuron, haloxyfop-P-methyl, and haloxyfop in tobacco leaf samples with high sensitivity has been established for the first time.

scholarly journals Simultaneous Determination of Acetylsalicylic Acid, Hydrochlorothiazide, Enalapril, and Atorvastatin in a Polypill-Based Quaternary Mixture by TLC

2018 ◽  
Vol 101 (3) ◽  
pp. 708-713
Author(s):  
Anna Maślanka ◽  
Mariusz Stolarczyk ◽  
Anna Apola ◽  
Anna Kwiecień ◽  
Urszula Hubicka ◽  
...  
Keyword(s):  
Acetylsalicylic Acid ◽  
Mobile Phase ◽  
High Sensitivity ◽  
Good Precision ◽  
Qualitative And Quantitative Analysis ◽  
Qualitative And Quantitative ◽  
Treatment And Prevention ◽  
Quaternary Mixture ◽  
Prevention Of Cardiovascular Disease

Abstract A new chromatographic-densitometric method has been developed for the qualitative and quantitative determination of the active ingredients in a simulated mixture corresponding to the PolyIran polypill, composed of acetylsalicylic acid, hydrochlorothiazide (HCT), enalapril (ENA), and atorvastatin (ATR), whose efficacy in the treatment and prevention of cardiovascular disease has been documented in clinical trials. Chromatographic separation was performed using TLC silica gel 60 plates with fluorescent indicator F254 as the stationary phase and a mixture of n-hexane–ethyl acetate–methanol–water–acetic acid (8.4 + 8 + 3 + 0.4 + 0.2, v/v/v/v/v) as the mobile phase. Densitometric measurements were carried out at λ = 210 nm when determining ENA and at λ = 265 nm in the case of the other drugs. Peaks of examined substances were well separated in the recorded chromatograms, enabling the evaluation of the results in terms of both qualitative and quantitative analysis. The method was specific for the analyzed components and was characterized by high sensitivity. The LOD was between 0.043 and 0.331 μg/spot, and LOQ was between 0.100 and 0.942 μg/spot. Recovery was in the range of 97.02–101.34%. The linearity range was broad and ranged from 0.600 to 6.000 μg/spot for acetylsalicylic acid, from 0.058 to 1.102 μg/spot for HCT, from 0.505 to 6.560 μg/spot for ENA, and from 0.100 to 1.000 μg/spot for ATR. The method was characterized by good precision, with RSD values that ranged from 0.10 to 2.26%.

scholarly journals Development and validation of a rapid selective high-throughput LC-MS/MS method for the determination of triclabendazole sulfoxide concentrations in sheep plasma and its use in bioequivalence studies

2021 ◽  
Author(s):  
Lénárd Farczádi ◽  
Álmos Dósa ◽  
Orsolya Melles ◽  
Laurian Vlase
Keyword(s):  
Formic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Liver Fluke ◽  
Internal Standard ◽  
Gradient Elution ◽  
Sample Processing ◽  
Development And Validation ◽  
Analytical Separation

AbstractTriclabendazole is one of the main drugs used to treat liver fluke in livestock. A rapid LC-MS/MS method was developed and validated to determine ovine plasma levels of triclabendazole sulfoxide.A Gemini NX-C18 column was used to achieve analytical separation, with gradient elution of a mobile phase composed of 0.1% formic acid in acetonitril and 0.1% formic acid in water at flow rate of 0.6 mL/min. MRM with positive ESI ionization was used for the detection of triclabendazole sulfoxide (m/z 360.10 from m/z 376.97). Fenbendazole was used as internal standard. Plasma protein precipitation with acetonitrile was used for sample processing.The method was validated with regards to selectivity, linearity (r > 0.9939), within run and between run precision (CV < 8.9%) and accuracy (bias < 8.9%) over the concentration range 1–100 µg/mL plasma.The method developed is simple, selective and can be applied in bioequivalence and bioavailability studies.

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