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.

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 and bioavailability of liensinine in mouse blood by UPLC-MS/MS

2020 ◽  
Author(s):  
Shuhua Tong ◽  
Yuqi Zeng ◽  
Jianshe Ma ◽  
Congcong Wen
Keyword(s):  
Pharmacokinetic Study ◽  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Quantitative Detection ◽  
Reaction Monitoring ◽  
Mouse Blood ◽  
Blood Samples ◽  
The Matrix ◽  
Better Than

AbstractLiensinine is a bisbenzyltetrahydroisoquinoline alkaloid extracted from lotus (Nelumbo nucifera GAERTNER., Nelumbonaceae), especially in its embryo loti “Lien Tze Hsin” (green embryo of mature seed). A rapid and simple UPLC-MS/MS method was developed to determine liensinine in mouse blood and its application to a pharmacokinetic study. The blood samples were preprocessed by protein precipitation using acetonitrile. Midazolam (internal standard, IS) and liensinine were gradient eluted by mobile phase of methanol and water (0.1% formic acid) in a Waters UPLC BEH C18 column. The multiple reaction monitoring of m/z 611.3 → 206.1 for liensinine and m/z 326.2 → 291.1 for IS with an electrospray ionization (ESI) source was used for quantitative detection. The calibration curve ranged from 0.5 to 400 ng/mL (r > 0.995). The accuracy ranged from 92.2 to 108.2%, the precision of intra-day and inter-day was less than 14%, and the matrix effect was between 100.0% and 109.6%, the recovery was better than 71.0%. The developed UPLC-MS/MS method was successfully used for a pharmacokinetic study of liensinine in mice after oral (5 mg/kg) and intravenous administration (1 mg/kg), and the absolute availability of liensinine was 1.8%.

Pharmacokinetic Study of Deltaline in Mouse Blood Based on UPLCMS/ MS

2019 ◽  
Vol 15 (2) ◽  
pp. 194-199 ◽  
Author(s):  
Huanchun Song ◽  
Yiwei Huang ◽  
Dongqing Zhu ◽  
Shuhua Tong ◽  
Meiling Zhang ◽  
...  
Keyword(s):  
Intravenous Administration ◽  
Pharmacokinetic Study ◽  
Internal Standard ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Mouse Blood ◽  
Limit Of Quantitation ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Precipitate Protein

Introduction: Deltaline, an aconitine-type alkaloid, was detected in mouse blood using an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method, and the pharmacokinetics of deltaline following intravenous administration in mice was studied. </P><P> Materials and Methods: The gelsenicine was used as the internal standard (IS). Deltaline and IS were eluted at a flow rate of 0.4 ml/min and separated on a UPLC BEH C18 column by gradient elution using acetonitrile and 10 mmol/L ammonium acetate (0.1% formic acid) as a mobile phase. The following transitions were obtained at m/z 508.2→75.0 for deltaline and m/z 327.1→107.8 for gelsenicine in multiple reactions monitoring mode. Acetonitrile was used to precipitate protein. Six mice after intravenous administration of a single dose of deltaline (1 mg/kg), 20-µL blood samples from each mouse were collected from the tail vein. Results: The UPLC-MS/MS method was sensitive and linear (r>0.995) with a lower limit of quantitation (LLOQ) of 0.1 ng/mL over the range of 0.1-500 ng/mL. Intra- and inter-day precisions were below 13%, the accuracy range was between 88.0% and 108.2%, the recovery was higher than 90.1%, and the matrix effect was between 102.9% and 108.1%. Conclusion: The method was sensitive, fast, specific, and has been successfully applied to a pharmacokinetic study of deltaline after intravenous administration.

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 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 A Novel UPLC-MS/MS Assay for the Measurement of Linezolid and its Metabolite PNU-142300 in Human Serum and its Application to Patients With Renal Insufficiency

2021 ◽  
Vol 12 ◽  
Author(s):  
Yingying Wang ◽  
Er-min Gu ◽  
Xiaoxiang Du ◽  
Ren-ai Xu ◽  
Guanyang Lin
Keyword(s):  
Liquid Chromatography ◽  
Renal Insufficiency ◽  
Human Serum ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Serum Samples ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

The contribution of the metabolites of linezolid to the associated myelosuppression is unknown in patients who are renal impairment. In this research, the purpose of our experiment was to explore and develop a quick and robust ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) assay for the determination of linezolid and its metabolite PNU-142300 in human serum simultaneously. The analytes were prepared using a simple and convenient approach with acetonitrile for protein crash, and then separated from the matrix on a Waters Acquity Ultra performance liquid chromatography (UPLC) BEH C18 (2.1 mm × 50 mm, 1.7 μm) column in a program of gradient elution, where the mobile phase was consisted of water with 0.1% formic acid and acetonitrile, and was placed at 0.40 ml/min flow rate. Multiple reaction monitoring (MRM) was employed and conducted for UPLC-MS/MS detection with ion transitions at m/z 338.01 → 296.03 for linezolid, m/z 369.96 → 327.98 for PNU-142300 and m/z 370.98 → 342.99 for tedizolid (Internal standard, IS), respectively. This method had good linearity respectively in the calibration range of 0.01–20 μg/ml for linezolid, and 0.05–100 μg/ml for PNU-142300. In the intra- and inter-day, the precision of linezolid and PNU-142300 was below 14.2%, and the accuracy in this method was determined to be from −9.7 to 12.8%. In addition, recovery and matrix effect of the analytes were all found to be acceptable, and the analytes during the assay and storage in serum samples were observed to be stable. The novel optimized UPLC-MS/MS assay was also successfully employed to determine the concentration levels of linezolid and PNU-142300 in human serum. The results showed that linezolid-associated myelosuppression occurs more frequently in patients with renal insufficiency, and the metabolite-to-parent concentration ratio of PNU-142300 is predicted to reduce this toxicity of myelosuppression.

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%.

scholarly journals Simultaneous Determination of Ropivacaine and 3-Hydroxy Ropivacaine in Cerebrospinal Fluid by UPLC-MS/MS

2020 ◽  
Vol 2020 ◽  
pp. 1-6
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Quan Zhou
Keyword(s):  
Cerebrospinal Fluid ◽  
Extraction Efficiency ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Reaction Monitoring ◽  
Limit Of Quantification ◽  
Liquid Liquid Extraction ◽  
The Matrix ◽  
Interday Precision

In this paper, a UPLC-MS/MS method was developed for the determination of ropivacaine and its metabolite 3-hydroxy ropivacaine in cerebrospinal fluid. The cerebrospinal fluid was processed by ethyl acetate liquid-liquid extraction. The multiple reaction monitoring (MRM) mode was used for quantitative analysis by monitoring the transitions of m/z 275.3 → 126.2 for ropivacaine, m/z 291.0 → 126.0 for 3-hydroxy ropivacaine, and m/z 290.2 → 198.2 for the internal standard. Standard curves for ropivacaine and 3-hydroxy ropivacaine in cerebrospinal fluid were conducted over the concentration range of 0.2–2000 ng/mL, demonstrating excellent linearity, and the lower limit of quantification was 0.2 ng/mL. The intraday precision of ropivacaine and 3-hydroxy ropivacaine was less than 11%, while the interday precision was less than 7%. The accuracy ranged between 87% and 107%, the average extraction efficiency was higher than 79%, and the matrix effect was between 89% and 98%. The developed method was then applied to a case of suspected poisoning of ropivacaine.

scholarly journals Pharmacokinetics of Lusutrombopag, a Novel Thrombopoietin Receptor Agonist, in Rats by UPLC-MS/MS

2020 ◽  
Vol 2020 ◽  
pp. 1-6
Author(s):  
Bo Wang ◽  
Feifei Chen ◽  
Quan Zhou ◽  
Yunfang Zhou ◽  
Deru Meng ◽  
...  
Keyword(s):  
Receptor Agonist ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Mass Spectrometric Measurement ◽  
Thrombopoietin Receptor ◽  
Positive Ion

Lusutrombopag is a second oral thrombopoietin (TPO) receptor agonist that selectively acts on human TPO receptors. In the study, UPLC-MS/MS was used to establish a selective and sensitive method to determine lusutrombopag with poziotinib as IS (internal standard) in rat plasma. Samples were prepared by precipitating protein with acetonitrile as a precipitant. Separation of lusutrombopag and poziotinib was performed on a CORTECS UPLC C18 column (2.1 ∗ 50 mm, 1.6 μm). The mobile phase (acetonitrile and water containing 0.1% formic acid) with gradient elution was set at a flow rate of 0.4 ml/min. The mass spectrometric measurement was conducted under positive ion mode using multiple reaction monitoring (MRM) of m/z 592.97 ⟶ 491.02 for lusutrombopag and m/z for poziotinib (IS) 492.06 ⟶ 354.55. The linear calibration curve of the concentration range was 2–2000 ng/ml for lusutrombopag, with a lower limit of quantification (LLOQ) of 2 ng/ml. RSD of interday and intraday precision were both no more than 9.66% with the accuracy ranging from 105.82% to 108.27%. The extraction recovery of lusutrombopag was between 82.15% and 90.34%. The developed and validated method was perfectly used in the pharmacokinetic study of lusutrombopag after oral administration in rats.

scholarly journals Development and Validation of an HPLC-MS/MS Method for Rapid Simultaneous Determination of Cefprozil Diastereomers in Human Plasma

2018 ◽  
Vol 2018 ◽  
pp. 1-9 ◽  
Author(s):  
Guodong He ◽  
Liping Mai ◽  
Xipei Wang
Keyword(s):  
Mass Spectrometry ◽  
Antimicrobial Activity ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Reaction Monitoring ◽  
Reverse Phase ◽  
Development And Validation ◽  
Positive Ion ◽  
Sensitive Method

Background. Both cis- and trans-cefprozil have antimicrobial activity, but their potencies are quite different. It is therefore necessary to develop a sensitive method to simultaneously determine both isomers for pharmacokinetic and bioequivalence studies. Methods. An LC-MS/MS method, using stable isotope-labeled cefprozil as the internal standard, was developed and validated. The analytes were extracted from plasma by protein precipitation and separated on a reverse-phase C18 column using a gradient program consisting of 0.5% formic acid and acetonitrile within 4 min. The mass spectrometry acquisition was performed with multiple reaction monitoring in positive ion mode using the respective [M+H]+ ions, m/z 391.2→114.0 for cefprozil and 395.0→114.5 for cefprozil-D4. Results. The calibration curves were linear over the ranges of 0.025–15 μg/mL for cis-cefprozil and 0.014–1.67 μg/mL for trans-cefprozil. The accuracies for the cis and trans isomers of cefprozil were 93.1% and 103.0%, respectively. The intra- and interassay precisions for the QC samples of the isomers were < 14.3%. The intra- and interassay precisions at the LLOQ were < 16.5%. Conclusions. The method was sensitive and reproducible and was applied in a pilot pharmacokinetic study of healthy volunteers.

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