scholarly journals Enantioseparation and Determination of Penconazole in Rat Plasma by Chiral LC-MS/MS: Application to a Stereoselective Toxicokinetic Study

Molecules ◽  
2020 ◽  
Vol 25 (13) ◽  
pp. 2964
Author(s):  
Siman Ma ◽  
Jia Lun ◽  
Yanru Liu ◽  
Zhen Jiang ◽  
Xingjie Guo
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Rat Plasma ◽  
Male Rats ◽  
Ionization Source ◽  
Established Method ◽  
Relative Standard

In this study, a specific and sensitive method of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the determination of penconazole enantiomers in rat plasma. The enantioseparation was achieved on a Chiralpak IC column by using acetonitrile/water (80:20, v/v) as the mobile phase. Penconazole enantiomers and internal standard l-lansoprazole (IS) were detected in multiple reaction monitoring (MRM) mode with positive electrospray ionization source. The method was validated over the concentration range of 2.5–250.0 ng mL−1 for penconazole enantiomers. Good linearity was obtained for both enantiomers with correlation coefficients (R) greater than 0.995. The relative error was well within the admissible range of −1.1–3.2%, and relative standard deviation was less than 6.0%. After validation, the established method was successfully applied to a stereoselective toxicokinetic study in female and male rats after oral administration of 50 mg kg−1 racemic penconazole. This is the first experiment regarding the stereospecific toxicokinetic study of penconazole and the bioanalytical approach for its quantitation in vivo.

scholarly journals A Validated HPLC-MS/MS Method for Simultaneous Determination of Militarine and Its Three Metabolites in Rat Plasma: Application to a Pharmacokinetic Study

2019 ◽  
Vol 2019 ◽  
pp. 1-9 ◽  
Author(s):  
Hui-Yuan Sun ◽  
Lin Zheng ◽  
Zi-Peng Gong ◽  
Yue-Ting Li ◽  
Chang Yang ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Area Under The Curve ◽  
Internal Standard ◽  
Rat Plasma ◽  
Relative Standard ◽  
Method Accuracy

A rapid, reliable, and sensitive HPLC-electrospray ionization-tandem mass spectrometry (HPLC-MS/MS) method was established and validated for simultaneous determination of militarine and its three metabolites (gastrodin, α-isobutylmalic acid, and gymnoside I) in rat plasma. Plasma was acidified with formic acid, and protein was precipitated with methanol. MS/MS with ESI and multiple reaction monitoring at m/z 725.3→457.3, 457.1→127, 304.3→107.2, 189→129, and 417.1→267.1 was used for determination of militarine, gastrodin, α-isobutylmalic acid, gymnoside I, and puerarin (internal standard), respectively. Chromatographic separation was conducted using an ACE UltraCore SuperC18 (2.1 × 100 mm, 2.5 μm) column with gradient mobile phase (0.1% formic acid in water and acetonitrile). The lower limits of quantitation for militarine, gastrodin, α-isobutylmalic acid, and gymnoside I were 1.02, 2.96, 1.64, and 0.3 ng/mL, respectively. The relative standard deviations of intra- and interday measurements were less than 15%, and the method accuracy ranged from 87.4% to 112.5%. The extraction recovery was 83.52%-105.34%, and no matrix effect was observed. The three metabolites (gastrodin, α-isobutylmalic acid, and gymnoside I) were synchronously detected at 0.83 h, suggesting that militarine was rapidly transformed to gastrodin, α-isobutylmalic acid, and gymnoside I. Moreover, the area under the curve (AUC) and Cmax of militarine were significantly lower than those of gastrodin and α-isobutylmalic acid, showing that militarine was largely metabolized to gastrodin and α-isobutylmalic acid in vivo. The studies on pharmacokinetics of militarine and its three metabolites were of great use for facilitating the clinical application of militarine and were also highly meaningful for the potential development of militarine.

scholarly journals UPLC–MS/MS simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, MDMA, and MDA in hair

2020 ◽  
Vol 32 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Peiwu Geng
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Ammonium Hydroxide ◽  
Ultra Performance Liquid Chromatography ◽  
Acetate Solution ◽  
Hair Samples ◽  
Relative Standard

Hair is a stable specimen and has a longer detection window (from weeks to months) than blood and urine. Through the analysis of hair, the long-term information of the drug use of the identified person could be explored. Our work is to establish an ultra-performance liquid chromatography–tandem mass spectroscopy (UPLC–MS/MS) method for simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in hair. Methoxyphenamine was used as an internal standard. The chromatographic separation was performed on a UPLC ethylene bridged hybrid (BEH) C18 (2.1 mm × 50 mm, 1.7 μm) column using a mobile phase of acetonitrile–water with 10 mmol/L ammonium acetate solution which containing 0.05% ammonium hydroxide. The multiple reaction monitoring in positive electrospray ionization was used for quantitative determination. The intra-day and inter-day precisions (relative standard deviation [RSD]) were below 15%. The accuracy ranged between 85.5% and 110.4%, the average recovery rate was above 72.9%, and the matrix effect ranged between 92.7% and 109.2%. Standard curves were in the range of 0.05–5.0 ng/mg, and the correlation coefficients were greater than 0.995. The established UPLC–MS/MS method was applied to analyze the hair samples successfully.

scholarly journals Pharmacokinetic Comparison of Isoalantolactone and Alantolactone in Rats after Administration Separately by Optimization of an UPLC-MS2Method

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Renjie Xu ◽  
Mengyue Wang ◽  
Ying Peng ◽  
Xiaobo Li
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Sprague Dawley ◽  
Ionization Source ◽  
Fragment Ions ◽  
Sprague Dawley Rats ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Ion

Isoalantolactone and alantolactone are two major active ingredients that are present in many medicinal plants. In this study, a sensitive and rapid ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for determination of the two compounds in rat plasma, separately. In this method, an electrospray ionization source was applied and operated in positive ion mode; multiple reaction monitoring (MRM) was selected for quantification using target fragment ions 233.2→187.1 for isoalantolactone (alantolactone) and 245.1→189.1 for internal standard (IS). Retention time of the lactones and IS was within 3.0 min. Further calibration suggested a linear regression can be calculated within 2.5–500 ng/mL for isoalantolactone and 4–500 ng/mL for alantolactone. This method was used to compare the pharmacokinetic characteristics of isoalantolactone and alantolactone at a single dose of 5 mg/kg into male Sprague-Dawley rats by intravenous administration separately. The levels oft1/2, Kel, CL,Cmax, and AUC were significantly increased in the alantolactone group compared to isoalantolactone. These results suggested that isoalantolactone was distributed and eliminated more rapidly than alantolactone in rats when administered, respectively.

scholarly journals Determination of 5-nitro-2-furaldehyde as marker residue for nitrofurazone treatment in farmed shrimps and with addressing the use of a novel internal standard

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Qiang Wang ◽  
Xu-Feng Wang ◽  
Yong-Yuan Jiang ◽  
Zhi-Guang Li ◽  
Nan Cai ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Ionization ◽  
Ultrasonic Manipulation

AbstractWe developed a significantly improved ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of 5-nitro-2-furaldehyde (NF) as a surrogate using a novel internal standard for the detection of nitrofurazone. We used 2,4-dinitrophenylhydrazine derivatization and furfural as the internal standard. Derivatization was easily performed in HCl using ultrasonic manipulation for 5 min followed by liquid extraction using ethyl acetate. The samples were concentrated and purified using reverse phase and alumina cartridges in tandem. The derivatives were separated using a linear gradient elution on a C18 column with methanol and water as the mobile phase in negative ionization mode and multiple reaction monitoring. Under the optimized conditions, the calibration curves were linear from 0.2 to 20 μg/L with correlation coefficients >0.999. Mean recoveries were 80.8 to 104.4% with the intra- and inter-day relative standard deviations <15% at spiking levels of 0.1 to 10 μg/kg. The limits of detection and quantification were 0.05 and 0.1 μg/kg, respectively. This method is a robust tool for the identification and quantitative determination of NF in shrimp samples.

scholarly journals Sensitive Quantification of Liensinine Alkaloid Using a HPLC-MS/MS Method and Its Application in Microvolume Rat Plasma

2021 ◽  
Vol 2021 ◽  
pp. 1-10
Author(s):  
Fen Wei ◽  
Xilan Gou ◽  
Xiao Xu ◽  
Sicen Wang ◽  
Tao Bao
Keyword(s):  
Quality Control ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
In Vivo Studies ◽  
Coefficient Of Determination ◽  
Ionization Source ◽  
Limit Of Quantification ◽  
Positive Mode

Liensinine, an important alkaloid in lotus seed, exhibits multiple functions such as anti-AIDS, anticancer, antidepressant, and antihypertensive properties. In this study, a highly sensitive HPLC-MS/MS method was developed and validated for the quantification of liensinine in microvolume rat plasma as low as 45 μL. Chromatographic separation was carried out using a reverse-phase Gemini-C18 column (100 mm × 3 mm i.d. × 5 μm), and mass selective detection using multiple reaction monitoring was attained using an electrospray ionization source, which operated in the positive mode. Dauricine was used as the internal standard. The precursor-to-product ion transition m/z 611.15 > 206.10 was selected for the detection of liensinine; m/z 625.25 > 206.10 was used for the detection of dauricine. The developed method is linear over the concentration range of 0.05–1000 ng/mL with an excellent coefficient of determination (R2 = 0.991). The recoveries ranged from 92.57% to 95.88% at three quality control levels. Intraday and interday precision and accuracy are less than 12.2% and 6.59%, respectively. The lower limit of quantification (LLOQ) is 0.05 ng/mL. The matrix effect was insignificant and acceptable. The validated method was successfully applied to the pharmacokinetic study of liensinine in rats. This method can be used for in vivo studies as well as quality control of traditional Chinese medicines and herbal tea containing liensinine alkaloid.

scholarly journals Development and Validation of a Sensitive UHPLC-MS/MS Method for the Measurement of Gardneramine in Rat Plasma and Tissues and its Application to Pharmacokinetics and Tissue Distribution Study

Molecules ◽  
2019 ◽  
Vol 24 (21) ◽  
pp. 3953 ◽  
Author(s):  
Zhao ◽  
Tan ◽  
Chen ◽  
Sun ◽  
Wang ◽  
...  
Keyword(s):  
Multiple Reaction Monitoring ◽  
Indole Alkaloid ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Limit Of Quantification ◽  
Tissue Samples ◽  
Distribution Study

As a novel monoterpenoid indole alkaloid, gardneramine has been confirmed to possess excellent nervous depressive effects. However, there have been no reports about the measurement of gardneramine in vitro and in vivo. The motivation of this study was to establish and validate a specific, sensitive, and robust analytical method based on UHPLC-MS/MS for quantification of gardneramine in rat plasma and various tissues after intravenous administration. The analyte was extracted from plasma and tissue samples by protein precipitation with methanol using theophylline as an internal standard (I.S.). The analytes were separated on an Agilent ZORBAX Eclipse Plus C18 column using a gradient elution of acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Gardneramine and I.S. were detected and quantified using positive electrospray ionization in multiple reaction monitoring (MRM) mode with transitions of m/z 413.1→217.9 for gardneramine and m/z 181.2→124.1 for I.S.. Perfect linearity range was 1–2000 ng/mL with a correlation coefficient (r2) of ≥0.990. The lower limit of quantification (LLOQ) of 1.0 ng/mL was adequate for application to different preclinical studies. The method was successfully applied for determination of gardneramine in bio-samples.

Simultaneous determination of five pesticides residues in Anoectochilus roxburghii by HPLC-MS/MS method

2020 ◽  
Vol 20 (5) ◽  
pp. 345-349
Author(s):  
Liqun WU ◽  
◽  
Mingke LUO ◽  
Wensheng HE ◽  
Wenting CHEN
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Acetonitrile Solution ◽  
Ionization Source ◽  
Thiophanate Methyl ◽  
Pesticides Residues ◽  
Relative Standard ◽  
Anoectochilus Roxburghii

Objective： To establish a HPLC-MS/MS method for simultaneous determination of five pesticides residues including tebuconazole，metalaxyl-M，thiophanate-methyl，oxytetracycline and abamectin in Anoectochilus roxburghii.Methods： The samples were extracted by acetonitrile solution and purified by QuEChERS method.Separation was performed on Agilent Eclipse Plus C18 column（50 mm×2.1 mm，1.8 μm） with the mobile phase consisting of 0.1% formic acid（A） and acetonitrile（B） by gradient elution（0-1.0 min，90% A；1.0-3.0 min，90%-70% A;3.0-5.0 min，70%-30% A;5.0-8.0 min，30%-10% A;8.0-14.0 min，10% A;14.0-15.0 min，10%-90% A;15.0-17.0 min，90% A）.Detection was performed on a triple quadrupole tandem mass spectrometry with electrospray ionization source operating in positive ion mode under multiple reaction monitoring（MRM） mode.Results： The calibration curves of five pesticides showed good linearity coefficients（r>0.99）.The average recoveries ranged from 72.7% to 94.9%（n=6），and the relative standard derivations（RSDs） were within 1.8%-10.3%（n=6）.The detection limits of tebuconazole，metalaxyl-M，thiophanate-methyl，oxytetracycline and abamectin were 0.6，0.2，0.3，0.2，5.0 μg/kg，and the quantitation limits of 5 pesticides were 2.0，0.5，1.0，0.6 and 10.0 μg/kg respectively.Conclusion： The established method was proved to be sensitive，simple and reliable，and could be applied for the determination of these five pesticides in Anoectochilus roxburghii and quality control in the planting process.

scholarly journals Development of a rapid UPLC-MS/MS method for the determination of toddalolactone in mouse blood and its application in pharmacokinetics

2021 ◽  
Author(s):  
Jing Zhou ◽  
Hongzhe Wang ◽  
Caiyun Miao ◽  
Yunxi Yao ◽  
Jianshe Ma
Keyword(s):  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Absolute Bioavailability ◽  
Quantitative Detection ◽  
Ionization Source ◽  
Mouse Blood ◽  
The Matrix ◽  
Product Ions

AbstractA rapid and simple UPLC-MS/MS method was developed to determine toddalolactone in mouse blood and applied to measure the pharmacokinetics of toddalolactone in mice. Blood samples were first preprocessed by ethyl acetate liquid-liquid extraction. Oxypeucedanin hydrate (internal standard, IS) and toddalolactone were gradient eluted from a UPLC BEH C18 column using a mobile phase consisting of acetonitrile and water (0.1% formic acid). Using electrospray ionization (ESI) as the ionization source, multiple reaction monitoring was used to detect the precursor and product ions of m/z 309.2 and 205.2, respectively, for toddalolactone and of m/z 305.1 and 203.0 for IS, respectively, for quantitative detection. A calibration curve was run over the concentration range of 5–4,000 ng/mL (r > 0.995). The matrix effects ranged from 93.5 to 98.4%, and the recovery was higher than 77.3%. The precision was less than 13%, and the accuracy ranged from 90.9 to 108.4%. The developed UPLC-MS/MS method was successfully used for measuring the pharmacokinetics of toddalolactone in mice after oral (20 mg/kg) and intravenous administration (5 mg/kg), and the absolute bioavailability of toddalolactone was 22.4%.

LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY/MASS SPECTROMETRY METHOD FOR THE DETERMINATION OF LAPATINIB IN RAT PLASMA: APPLICATION TO PHARMACOKINETIC STUDIES IN WISTAR RATS

2021 ◽  
pp. 74-77
Author(s):  
NARMADA PALNATI ◽  
NALINI KOTAPATI ◽  
GOPAL VAIDYANATHAN
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Wistar Rats ◽  
Internal Standard ◽  
Rat Plasma ◽  
Liquid Chromatography Mass Spectrometry ◽  
Tertiary Butyl ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

Objective: The objective of the study was to develop and validate a simple, accurate, and sensitive liquid chromatography–mass spectrometry (LC–MS)/MS method for the determination of lapatinib a dual tyrosine kinase inhibitor in rat plasma using gefitinib as internal standard. Methods: An Inertsil ODS column (50 mm×4.6 mm×5 μm) was used for separation with isocratic elution of 10 mM ammonium formate-acetonitrile (5:95 v/v). Analyte and internal standard were extracted from 50 μl of plasma using tertiary butyl methyl ether followed by subsequent reconstitution in a mixture of water-acetonitrile. Results: The extraction recoveries were 95% and 98% for lapatinib and gefitinib, respectively. The lower limit of quantification was 5 ng/ml with a precision of 6.2% and accuracy of 108%. The response was found to be linear over the range of 5–1000 ng/ml with a correlation coefficient of 0.999. The intraday and interday precision expressed as relative standard deviation was <15%. Conclusion: This validated method was applied to the pharmacokinetic study in Wistar rats. The proposed bioanalytical LC–MS/MS method for lapatinib is a simple, sensitive, and accurate to quantify the concentrations in rat plasma.

scholarly journals Hollow fibre liquid phase microextraction of parabens

2009 ◽  
Vol 7 (3) ◽  
pp. 285-290 ◽  
Author(s):  
Aleksandra Prichodko ◽  
Kristina Jonusaite ◽  
Vida Vickackaite
Keyword(s):  
Liquid Phase ◽  
Urine Analysis ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Chromatographic Determination ◽  
Enrichment Factors ◽  
Hollow Fibre ◽  
Liquid Phase Microextraction ◽  
Relative Standard

AbstractA hollow fibre liquid phase microextraction for gas chromatographic determination of some p-hydroxybenzoic acid esters has been developed. Chlorobenzene containing tetradecane as internal standard was used for the extraction. Optimized extraction was carried out at room temperature for 40 min in the presence of 0.4 g mL−1 NaCl in the sample solution. Calibration was linear up to 30 mg L−1. Correlation coefficients were 0.996–0.998. Enrichment factors were 21, 95 and 154, and detection limits were 0.20, 0.03 and 0.01 μg mL−1 for methylparaben, ethylparaben and propylparaben, respectively. Reproducibility was acceptable with relative standard deviations up to 11.7%. The technique was tested for water and urine analysis.

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