scholarly journals The Effect of Tanreqing Injection on the Pharmacokinetics of Sirolimus in Rats

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Feng Zhang ◽  
Liang Sun ◽  
Jianxiu Zhai ◽  
Tianyi Xia ◽  
Wei Jiang ◽  
...  
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
Matrix Effects ◽  
Thaw Cycle ◽  
Relative Standard ◽  
The Matrix ◽  
Freeze Thaw Cycle ◽  
Liquid Chromatography Tandem Mass ◽  
The Stability ◽  
First Time

To evaluate the effect of Tanreqing injection on the pharmacokinetics of sirolimus in rats, a high performance liquid chromatography tandem mass spectrometry method was developed for sirolimus assay in whole blood. Calibration curve of sirolimus was acquired over a concentration ranging from 2.5 to 100 ng/mL with r2= 0.9955. The matrix effects and extraction recoveries of sirolimus ranged from 144% to 152% and from 80% to 96%, respectively. The inter- and intraday relative standard deviations were both <10%. The stability investigation showed that the blood samples were stable for 30-day-storage at -20°C, for 8 h storage at room temperature, for 24 h storage in the auto-sampler at 4°C, and for three freeze-thaw cycle process. The pharmacokinetic results demonstrated that the Cmax, AUC, and AUMC of sirolimus in rats (7.5 mg/kg, i.g.) were increased after beincoadministration with Tanreqing Injection at 2.5, 5.0, and 7.5 mL/kg (i.v.), respectively, or at 5 min, 2 h, and 4 h (5.0 mL/kg, i.v.) after SRL dosing, respectively. For the first time, the results proved the herb-drug interaction between Tanreqing Injection and sirolimus and accordingly suggested avoiding concurrent reception of those two drugs for patients.

Fully-Automated SPE Coupled to UPLC-MS/MS Method for Simultaneous Detection of Trace Sulfonamides, Quinolones, and Macrolide antibiotics in Water

2021 ◽  
Author(s):  
Ming Zheng ◽  
Suwen Tang ◽  
Yangyang Bao ◽  
Kevin D Daniels ◽  
Zuo Tong How ◽  
...  
Keyword(s):  
High Performance ◽  
Matrix Effects ◽  
Solid Phase ◽  
Yangtze River Basin ◽  
Pure Water ◽  
Simultaneous Detection ◽  
Sample Volume ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

Abstract A fully automated solid-phase extraction (SPE) coupled ultra-high-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed for analysis of antibiotics (sulfonamides, quinolones, and macrolide) in water matrices. Sample preparation optimization included the selection of the best SPE material and configuration (HLB disks), sample volume (500−1000 mL water sample (pH = 3)) with a flow rate at 1−2 mL min− 1, and an elution procedure with 2 ⋅ 6 mL methanol, 2 ⋅ 6 mL acetone-methanol (V/V = 1/1). Meanwhile, the parameters for UPLC-MS/S detection of each analyte was optimized, including LC retention time, and MS parameters. The instrumental limits of detection (LOD) and quantification (LOQ) of analytes ranged from 0.01−0.72 µg L− 1 and 0.05−2.39 µg L− 1, respectively, with good linear correlation (R2 > 0.995) and precision (< 9.9%). Matrix spike recoveries ranged between 63.3−99.2% in pure water, 60.8−91.3% in surface water (SW), and 59.9−102.8% in wastewater effluent (WWE) with relative standard deviations (RSD) below 11%. The matrix effects (MEs) observed for most of the analytes were ion suppression (0−25.8%) except for four compounds that had enhancement (0−8.0 %) in SW or WWE. This method can basically meet the needs of trace antibiotic residues detection in waters. Trace levels of sulfonamides, quinolones and macrolides using the developed antibiotic method were below LOQ (BQL) −94.47 ng L− 1 in WWEs and BQL−15.47 ng L− 1 in SW in the lower reaches of the Yangtze River Basin.

The Effect of Freeze/Thaw Cycles on the Stability of Compounds in DMSO

2003 ◽  
Vol 8 (2) ◽  
pp. 210-215 ◽  
Author(s):  
Barbara A. Kozikowski ◽  
Thomas M. Burt ◽  
Debra A. Tirey ◽  
Lisa E. Williams ◽  
Barbara R. Kuzmak ◽  
...  
Keyword(s):  
High Throughput Screening ◽  
High Performance ◽  
Atmospheric Conditions ◽  
Freeze Thaw ◽  
Thaw Cycle ◽  
Time Period ◽  
Freeze Thaw Cycle ◽  
Low Humidity ◽  
The Stability ◽  
Short Time

A diverse set of 320 compounds from the Procter & Gamble Pharmaceuticals organic compound repository was prepared as 20-mM DMSO solutions and stored at 4°C under argon in pressurized canisters to simulate a low-humidity environment. The plates were subjected to 25 freeze/thaw cycles while being exposed to ambient atmospheric conditions after each thaw to simulate the time and manner by which compound plates are exposed to the atmosphere during typical liquid-handling and high-throughput screening processes. High-performance liquid chromatography–mass spectrometry with evaporative light-scattering detection was used to quantitate the amount of compound remaining after every 5th freeze/thaw cycle. Control plates were stored either at room temperature under argon or at 4°C under argon without freeze/thaw cycling and were evaluated at the midpoint and the endpoint of the study. The study was conducted over a short time period (i.e., 7 weeks) to minimize the effect of compound degradation over time due to the exposure of the compounds to DMSO.The results from this study will be used to determine the maximum number of freeze/thaw cycles that can be achieved while maintaining acceptable compound integrity.(Journal of Biomolecular Screening 2003:210-215)

Multitemperature Stability and Degradation Characteristics of Pergolide Mesylate Oral Liquid

2010 ◽  
Vol 23 (6) ◽  
pp. 570-574 ◽  
Author(s):  
Brandon R. Shank ◽  
Clyde M. Ofner
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
Color Change ◽  
Degradation Process ◽  
First Order ◽  
Drug Concentrations ◽  
Relative Standard ◽  
Oral Liquid ◽  
The Stability ◽  
Initial Drug

The stability of pergolide mesylate in an oral aqueous liquid was studied. Stability and solubility data were used to determine the degradation characteristics of the drug in this formulation. Samples were stored in the dark at 35°C, 45°C, and 60°C. At 1, 2, 4, 8, 12, and 16 weeks, samples were removed and stored in a −80°C freezer for high performance liquid chromatography (HPLC) assay at a later date. The initial drug concentration of 0.30 mg/mL was determined by assay after storage at −80°C. A solubility of 6.9 mg/mL was found for pergolide mesylate in the oral liquid at room temperature with a relative standard deviation (RSD) of 4.0%. The degradation process is considered first-order at 25°C and 35°C. At higher temperatures (45°C and 60°C), a color change and curvature at the latter time points in degradation profiles are ascribed to the presence of methylcellulose. The activation energy calculated for degradation of pergolide mesylate in the oral liquid was 21.3 kcal/mol. The time to reach 90% potency (t90) values were calculated to be 43 days and 3 days, respectively, for storage at 25°C and 35°C. Drug concentrations up to ~6 mg/mL can be maintained as a solution at room temperature with this formulation.

scholarly journals Isothiazolinones Quantification in Shampoo Matrices: A Matter of Method Optimization or Stability Driven by Interactions?

Cosmetics ◽  
2020 ◽  
Vol 7 (1) ◽  
pp. 4
Author(s):  
Mariana Tomás ◽  
Ana Sofia Agonia ◽  
Lígia Borges ◽  
Ana Palmeira de Oliveira ◽  
Rita Palmeira de Oliveira
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
Extraction Procedure ◽  
Magnesium Silicate ◽  
Array Detector ◽  
Diode Array Detector ◽  
The Matrix ◽  
Method Optimization ◽  
Formulation Factors ◽  
The Stability

Methylisothiazolinone (MI) is one of the most used preservatives in shampoos and also one of the most effective. A preservative mixture known as Kathon™ CG is commercially available. It contains 5-chloro-2-methyl-4-isothiazolin-3-one (CMI) and 2-methyl-4-isothiazolin-3-one (MI) (3:1) and stabilizers. The aim of this study is to evaluate the influence of formulation factors in the quantification and stability of isothiazolinones in shampoos. Two shampoo bases containing Kathon™ CG as a preservative were prepared. Some ingredients that are at risk of interfering with the preservative stability were added to these formulations. The preservative was quantified by HPLC-DAD (High-performance liquid chromatography with a diode-array detector) after preparation of the formulation and after storage at room temperature and at 40 °C. The addition of magnesium silicate proved to be essential for the breakdown of the interaction between the matrix and the analytes in the extraction procedure. The content of CMI/MI decreased right after preparation indicating that immediate interactions between CMI/MI and the ingredients may have occurred after preparation resulting in a decrease in the preservative concentration. Detrimental interactions between the ingredients, regarding the stability of the isothiazolinones were detected immediately after preparation and over time resulting in the reduction of CMI/MI concentration in these cosmetic shampoos.

Phenotyping of Hyperlipoproteinemias

1970 ◽  
Vol 16 (6) ◽  
pp. 507-511 ◽  
Author(s):  
James Winkelman ◽  
Donald R Wybenga ◽  
Frank A Ibbott
Keyword(s):  
Cellulose Acetate ◽  
Room Temperature ◽  
Cellulose Acetate Electrophoresis ◽  
Freeze Thaw ◽  
Thaw Cycle ◽  
Freeze Thaw Cycle ◽  
The Stability

Abstract The stability of serum specimens collected for cellulose acetate electrophoresis of lipoproteins has been studied for each of the hyperlipoproteinemia phenotypes. In general, samples kept at room temperature for three days are still suitable for analysis. On longer standing, artifacts can cause misinterpretation of strips, or render them completely unreadable. If specimens are stored at refrigerator or freezer temperatures, deterioration is retarded but the period of stability after they are returned to room temperature is unaltered. A second freeze-thaw cycle makes specimens unsuitable for analysis. Samples can be stored at refrigerator temperatures for at least 28 days and at freezer temperatures for at least 14 days if one freeze-thaw cycle is used.

Single-Laboratory Validation of a Multi-residue Method for Simultaneous Analysis of Multi-class Pesticides in Turmeric by Liquid Chromatography Tandem Mass Spectrometry

2020 ◽  
Author(s):  
Bappa Ghosh ◽  
Arijita Bhattacharyya ◽  
Sandip Hingmire ◽  
Pushpa Aher ◽  
Pradnya Zende ◽  
...  
Keyword(s):  
Matrix Effects ◽  
Solid Phase ◽  
Residue Analysis ◽  
High Throughput Analysis ◽  
Method Performance ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Powder Samples ◽  
First Time

Abstract Background For years, turmeric has been used in several cuisines worldwide because of its proven health benefits. However, as its cultivation often involves applications of polar and semi-polar pesticides, their residues might cause health hazards to consumers. The dearth of a validated LC-MS/MS method for the residue analysis of these pesticides in turmeric has warranted the present study. Objective The aim was to develop and validate a multi-residue method for simultaneous determination of multi-class pesticides in turmeric (both rhizome and powder) by LC-MS/MS. Method Both the rhizome and powder samples (1 kg) were soaked in water for 30 min, followed by homogenization. Each homogenate (2 g) was mixed with 10 mL water, and extracted with acetonitrile (10 mL) in the presence of acetic acid and NaCl. The extract was cleaned by using dispersive solid phase extraction (dSPE) with graphitized carbon (5 mg/mL) sorbent. The cleaned extract was measured by LC-MS/MS with a runtime of 20 min. The method was validated on 211 multi-class pesticides. Results The method performance was satisfactory at 10 ng/g and higher levels, in compliance with the SANTE/12682/2019 guidelines. The dSPE cleanup was effective in minimizing the matrix effects. The use of matrix-matched calibrations specific for turmeric powder and rhizome corrected all recoveries within the satisfactory range of 70–120%. The precision -RSDs were &lt;20% for all test pesticides. The Horwitz ratio and measurement uncertainty results were satisfactory as well. Conclusions As the method was convenient, selective, accurate, and repeatable, it is recommended for regulatory and commercial testing purposes. Highlights For the first time, this study reports a validated LC-MS/MS method for the multi-residue analysis of pesticides in turmeric. The method provided a high throughput analysis of multi-class pesticides in turmeric rhizome and powder matrices with satisfactory selectivity, sensitivity, accuracy, and precision. The method performance satisfied the requirements of the SANTE/12682/2019 guidelines, and the method sensitivity complied with the EU-MRL requirements.

scholarly journals Simultaneous Determination of Five Components of Chaihu-Shugan-San in Beagle Plasma by HPLC-MS/MS and Its Application to a Pharmacokinetic Study after a Single Dose of Chaihu-Shugan-San

2020 ◽  
Vol 2020 ◽  
pp. 1-11
Author(s):  
Yong-liang Zhu ◽  
Hui-jun Wang ◽  
Hao Xue ◽  
Yi Zhang ◽  
Qian-shi Cheng ◽  
...  
Keyword(s):  
Single Dose ◽  
High Performance ◽  
Matrix Effects ◽  
Gradient Elution ◽  
Gastrointestinal Diseases ◽  
Column Temperature ◽  
Mobile Phases ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Total Measurement Time

Chaihu-shugan-san (CHSGS) has been widely used in China to treat depression and gastrointestinal diseases for thousands of years, but little is known about its pharmacokinetic properties. The purpose of our study is to develop a reliable and sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method to detect five components in beagle plasma and study their pharmacokinetic after oral administration of CHSGS in beagles. An Agilent C18 column (2.1 × 150 mm, 3.5 μm) was used to separate the analytes, and the column temperature was maintained at 40°C. A gradient elution procedure was used with solvent A (acetonitrile) and solvent B (0.1% formic acid, aqueous) as mobile phases. The elution procedure was 60% B—10% B (0–3 min) and 10% B—60% B (3.1–4 min). The flow rate was 0.3 mL/min, and the total measurement time was 4 min. Within the determined range, the standard calibration curves of the five analytes had a satisfactory linear relationship (r2 ≥ 0.9923). The recovery rate (n = 6) of the five analytes was between 85.42% and 90.85%, and the matrix effects (n = 6) were between 94.52% and 103.91%. These results show that the validated method could be successfully applied to study the pharmacokinetic in beagles after a single dose of CHSGS.

Development of an HPLC-UV Method for Quantification of Stattic

2019 ◽  
Vol 15 (6) ◽  
pp. 568-573
Author(s):  
Soheil Sedaghat ◽  
Ommoleila Molavi ◽  
Akram Faridi ◽  
Ali Shayanfar ◽  
Mohammad Reza Rashidi
Keyword(s):  
High Performance ◽  
Accurate Method ◽  
Plasma Samples ◽  
Promising Target ◽  
Relative Standard ◽  
Dimerization Inhibitor ◽  
Oncogenic Protein ◽  
First Time ◽  
Transcription 3

Background: Signal transducer and activator of transcription 3 (STAT3), an oncogenic protein found constitutively active in many types of human malignancies, is considered to be a promising target for cancer therapy. Objective: In this study for the first time, a simple and accurate method has been developed for the determination of a STAT3 dimerization inhibitor called stattic in aqueous and plasma samples. Methods: A reverse-phase high-performance liquid chromatography (RP-HPLC) composed of C18 column as stationary phase, and the mixture of acetonitrile (60%) and water (40%) as mobile phase with a UV detection at 215 nm were applied for quantification of stattic. The developed method was validated by Food and Drug Administration (FDA) guideline. Results: The method provided a linear range between 1-40 and 2.5-40 µg mL-1 for aqueous and plasma samples, respectively, with a correlation coefficient of 0.999. The accuracy (as recovery) of the developed method was found to be between 95-105% for aqueous medium and 85-115% for plasma samples. The precision (as relative standard deviation) for aqueous and plasma samples was less than 6% and 15%, respectively. The sensitivity of the developed method based on FDA guideline was 1 µg mL-1 for aqueous and 2.5 µg mL-1 for plasma samples. Conclusion: These results show that the established method is a fast and accurate quantification for stattic in aqueous and plasma samples.

scholarly journals Simplified and Rapid Determination of Primaquine and 5,6-Orthoquinone Primaquine by UHPLC-MS/MS: Its Application to a Pharmacokinetic Study

Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Rapid Determination ◽  
Active Metabolites ◽  
Chromatography Tandem Mass Spectrometry ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Isocratic Mode

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.

scholarly journals Development and Validation of a Sensitive, Specific and Reproducible UPLC-MS/MS Method for the Quantification of OJT007, A Novel Anti-Leishmanial Agent: Application to a Pharmacokinetic Study

2021 ◽  
Vol 18 (9) ◽  
pp. 4624
Author(s):  
Maria Rincon Nigro ◽  
Jing Ma ◽  
Ololade Tosin Awosemo ◽  
Huan Xie ◽  
Omonike Arike Olaleye ◽  
...  
Keyword(s):  
Formic Acid ◽  
High Performance ◽  
Leishmania Major ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Acquity Uplc

OJT007 is a methionine aminopeptidase 1 (MetAP1) inhibitor with potent anti-proliferative effects against Leishmania Major. In order to study its pharmacokinetics as a part of the drug development process, a sensitive, specific, and reproducible ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated. Voriconazole was used as the internal standard to generate standard curves ranging from 5 to 1000 ng/mL. The separation was achieved using a UPLC system equipped with an Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) with 0.1% formic acid in acetonitrile and 0.1% formic acid in water as the mobile phase under gradient elution at a flow rate of 0.4 mL/min. The mass analysis was performed with a 4000 QTRAP® mass spectrometer using multiple-ion reaction monitoring (MRM) in the positive mode, with the transition of m/z 325 → m/z 205 for OJT007 and m/z 350 → m/z 101 for voriconazole. The intra- and inter-day precision and accuracy were within ±15%. The mean extraction recovery and the matrix effect were 95.1% and 7.96%, respectively, suggesting no significant matrix interfering with the quantification of the drug in rat plasma. This study was successfully used for the pharmacokinetic evaluation of OJT007 using the rat as an animal model.

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