Screening of Synthetic Cathinones and Metabolites in Dried Blood Spots by UPLC–MS-MS

2020 ◽  
Author(s):  
Yang Wang ◽  
Yan Shi ◽  
Yingjia Yu ◽  
Lizhu Chen ◽  
Jiebing Jiang ◽  
...  
Keyword(s):  
Multiple Reaction Monitoring ◽  
Dried Blood Spots ◽  
Ultra Performance Liquid Chromatography ◽  
Sample Volume ◽  
Synthetic Cathinones ◽  
Limit Of Quantification ◽  
Blood Spots ◽  
Liquid Chromatography Tandem Mass ◽  
Ionization Mode ◽  
Acquity Uplc

Abstract After its use for decades in clinical screening, dried blood spots (DBS) have recently received considerable attention for their application in various novel psychoactive substances. The goal of this study was to develop and apply a DBS-based assay for 37 synthetic cathinones and their metabolites. Thirty microliters of whole blood sample after administration was spotted onto Whatman FTA classical cards, dried and extracted, and then analyzed by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS-MS). The samples were chromatographed on a Waters Acquity UPLC®HSS T3 column (1.8 μm, 2.1 × 100 mm) and then identically packed defender guard cartridges of a Waters Acquity UPLC®HSS T3 column (1.8 μm, 2.1 × 5 mm, 3/pk). The separation was achieved via solvents of 20 mM ammonium acetate/formic acid 0.1% (A) and acetonitrile (B) at a flow rate of 0.25 mL/min. A tandem MS equipped with positive electrospray ionization mode source was used as the detector. Multiple reaction monitoring with the precursor/product ion combinations was used to quantify each analyte. The linear range of synthetic cathinones in the DBS was 2.0–200 ng/mL, and the lowest limit of quantification was 2.0 ng/mL for some synthetic cathinones and 10 ng/mL for others. The precision and accuracy of the results for the validation samples of the synthetic cathinones were within acceptable criteria. DBS sampling offers the advantages of reduced sample volume and convenient sample storage and shipment. This method can be successfully applied to the quantification of synthetic cathinones.

An UPLC-MS/MS Method for Routine Quantification of Insulin Degludec in Plasma

2020 ◽  
Vol 16 (6) ◽  
pp. 792-799
Author(s):  
Yudong Zhang ◽  
Yue Jiang ◽  
Ya Wang ◽  
Ling Wang ◽  
Weijie Han ◽  
...  
Keyword(s):  
Formic Acid ◽  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Subcutaneous Administration ◽  
Ultra Performance Liquid Chromatography ◽  
Insulin Degludec ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Acquity Uplc

Background: Chromatographic methods for determination of insulin degludec in rabbit plasma by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry were developed. Methods: Analytes were eluted from Waters ACQUITY UPLC® Peptide BEH C18 (2.1×50mm, 300Å) column with a mobile phase of water containing 0.1% formic acid (A) and acetonitrile containing 0.1% formic acid (B). Quantitation of insulin degludec was performed using 1222.06 > 641.24 m/z on Multiple- Reaction Monitoring (MRM) mode. Results: Good linearity was observed in the concentration range of 500-50000 ng/mL (r >0.99), and the lower limit of quantification was 500ng/mL. The within-run and between-run precision (expressed as relative standard deviation, RSD) of insulin degludec were ≤ 14.16% and ≤ 13.64% respectively, and the accuracy was within 94.37-96.35%. The recovery and matrix effects were both within acceptable limits. Conclusion: This method was successfully applied for the pharmacokinetic study of insulin degludec in rabbit after subcutaneous administration.

scholarly journals P63 UPLC/MS/MS assay for the simultaneous determination of seven antibiotics in human serum – application to pediatric studies

2019 ◽  
Vol 104 (6) ◽  
pp. e43.2-e43
Author(s):  
S Magreault ◽  
O Chaussenery-Lorentz ◽  
T Storme ◽  
E Jacqz-Aigrain
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Routine Activity ◽  
Therapeutic Drug ◽  
Pharmacokinetic Studies ◽  
Pediatric Dose ◽  
Liquid Chromatography Tandem Mass ◽  
Sampling Volume ◽  
Acquity Uplc

BackgroundAntimicrobials are widely used in children but pediatric dose regimens are not always validated, and PK studies, required to validate dosage, are difficult to conduct in children. Low sampling volume limits the number of PK samples drawn per patient and analytical methods adapted to small volumes are not always available. Due to the wide inter-patient pharmacokinetic (PK) variability in children, particularly neonates, therapeutic drug monitoring is required to adapt dosage to individual patients. In such clinical and analytical context, our aim was to develop a unique, rapid and highly sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) assay to quantify 7 antibiotics (amoxicillin, azithromycin, cefotaxime, ciprofloxacin, meropenem, metronidazole and piperacillin) in low sample volumes (50 µL) for both routine monitoring and pharmacokinetic studies.MethodsAfter protein precipitation by acetonitrile, the antibiotics and their associated deuterated internal standard were separated on a Waters Acquity UPLC HSS T3 (100 mm x 2.1 mm; 1.8 µm). The mobile phases consisted of a gradient of ammonium acetate (pH 2.4; 5mM) and acetonitrile acidified with 0.1% (v/v) formic acid (started ratio of 93:7, v/v), run at 0.5 mL/min flow rate (total run time: 2.75 min). Ions were detected in the turbo-ion-spray-positive and multiple-reaction-monitoring modes.ResultsThis method was linear from 0.1–50 µg/mL. Accuracy and precision were evaluated using Quality Control (2, 10, 35 µg/mL). Validation of the method proved that precision, selectivity and stability were all within the recommended limits.ConclusionThis method has the advantage of a unique, efficient and standardized analytical tool for rapid measurement of 7 antibiotics in low blood volume. It has been successfully applied for routine activity and pharmacokinetic studies in children and neonates.Disclosure(s)Nothing to disclose.

Simultaneous Quantification of 38 Psychotropic Drugs and Relevant Metabolites in Blood using LC–MS-MS

2020 ◽  
Author(s):  
Rongzhe Zhu ◽  
Xiaoru Dong ◽  
Dingang Zhang ◽  
Xiaochen Liu ◽  
Yonghong Ye ◽  
...  
Keyword(s):  
Whole Blood ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Comprehensive Information ◽  
Practical Usefulness ◽  
Previous Medication ◽  
Liquid Chromatography Tandem Mass ◽  
Ionization Mode ◽  
Acquity Uplc ◽  
Blood Analytes

Abstract The trend for the concomitant prescription of antidepressants and antipsychotics is increasing. This calls for a veracious screening and quantifying method for forensic and clinical use. In this study, a liquid chromatography–tandem mass spectrometry (LC–MS-MS) method was developed and validated for the simultaneous determination and quantification of 38 antidepressants, antipsychotics and relevant metabolites in small volumes (200 μL) of human whole blood. Analytes and deuterated internal standards were extracted using liquid–liquid extraction. The separation, determination and quantification of the analytes were performed using an LC–MS-MS system equipped with an ACQUITY UPLC® BEH Phenyl Column under a positive electrospray ionization mode. After validation, the analytical procedure was proved to be highly sensitive, with a limit of detection ranging from 0.0005 to 1 ng/mL and a lower limit of quantification ranging from 0.002 to 2 ng/mL. Bias and within- and between-run precision were within 14.7% for all analytes. Recoveries were reproducible and those of 35 analytes were >50%. Dilution integrity was evaluated to ensure that the therapeutic and toxic blood concentration ranges of target compounds were fully covered. Finally, this method was applied to authentic whole blood samples collected from two forensic cases, which demonstrated its practical usefulness of providing accurate and comprehensive information concerning the previous medication of the deceased.

Validation of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Electrospray Ionization Method for Quantitative Determination of Ornidazole in Solid Dispersion

2020 ◽  
Vol 16 (5) ◽  
pp. 487-493
Author(s):  
Gopal Prasad Agrawal ◽  
Rajesh Kumar Maheshwari ◽  
Pradeep Mishra
Keyword(s):  
Method Validation ◽  
Solid Dispersion ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Ultra Performance Liquid Chromatography ◽  
Limit Of Quantification ◽  
Ionization Method ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode

Background and Objective: The present study describes the UPLC-MS/MS method validation for the analysis of ornidazole in solid dispersion. Methods: The proposed UPLC-MS/MS method utilizes BEH Shield RP18 column (2.1 mm 100 mm, 1.7 μm) with a gradient programmed mobile phase composed of water and acetonitrile at a flow rate of 0.4 mL/min which varies with time program. Ornidazole was detected by UPLC-MS/MS with three proton adducts at m/z 82.04, 128.05 as daughter ions and 220.03 as a parent ion in Multiple Reaction Monitoring (MRM) operated in positive mode. Results: Adducts at m/z 128.05 was found to be the most stable and showed higher intensity was selected for quantification of ornidaozle in solid dispersion. In the method, validation linearity was determined at concentration range of 10-100ng/mL and a correlation coefficient was found (r2) ≥0.9994. The limit of detection and limit of quantification were found to be 1.5 and 4 ng/mL, respectively. Inter and Intra-day precision was found within 0.33 and 0.11% and accuracy within 100.08% and 100.04%. Conclusion: A sensitive and selective UPLC-MS/MS method had been validated for the analysis of ornidazole in solid dispersion. The proposed method of analysis of ornidazole in solid dispersion can be used in quality control laboratories.

scholarly journals Pharmacokinetics of ebeiedinone in mouse blood by UPLC–MS/MS

2020 ◽  
Vol 32 (3) ◽  
pp. 194-198
Author(s):  
Yongxi Jin ◽  
Yuyan Chen ◽  
Jiawen Liu ◽  
Xi Bao ◽  
Yinghao Zhi ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Absolute Bioavailability ◽  
Mouse Blood ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was established to determine ebeiedinone in mouse blood, and the pharmacokinetics of ebeiedinone after intravenous (0.5 mg/kg) and oral (2, 4, and 8 mg/kg) administration was studied. Twenty-four mice were randomly divided into 4 groups, 1 group was for intravenous administration (0.5 mg/kg), and other 3 groups were for oral administration (2, 4, and 8 mg/kg), with 6 rats in each group. Yubeinine was used as an internal standard. Multiple reaction monitoring (MRM) mode was used to quantitatively analyzed ebeiedinone m/z 414.4 → 91.1 and the internal standard m/z 430.4 → 412.3 in the electrospray ionization (ESI) positive interface. In the concentration range of 1–2000 ng/mL, the ebeiedinone in the mouse blood was linear (r2 > 0.995), and the lower limit of quantification was 1.0 ng/mL. In the mouse blood, the intra-day precision coefficient of variation (CV) was less than 15%, and the inter-day precision CV was less than 15%. The accuracy ranged from 85.4% to 114.6%, and the average recovery was higher than 61.3%. The matrix effect was between 87.0% and 106.5%. These data met the pharmacokinetic study requirements of ebeiedinone. The UPLC–MS/MS method was sensitive, rapid, and selective and was successfully applied to the pharmacokinetic study of ebeiedinone in mice. The absolute bioavailability of ebeiedinone was 30.6%.

scholarly journals Quantitation ofα-Lactalbumin by Liquid Chromatography Tandem Mass Spectrometry in Medicinal Adjuvant Lactose

2014 ◽  
Vol 2014 ◽  
pp. 1-4 ◽  
Author(s):  
Rui Yan ◽  
Longmei Qu ◽  
Nan Luo ◽  
Yang Liu ◽  
Yu Liu ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Selected Ion Monitoring ◽  
Limit Of Quantification ◽  
Technical Preparation ◽  
Liquid Chromatography Tandem Mass ◽  
Ionization Mode ◽  
Acquity Uplc

Lactose is a widely used pharmaceutical excipient, sometimes irreplaceable. Traces of residual proteins left during production of lactose are potential allergen to body. The present paper describes a sensitive and specific LC-MS method for the determination ofα-lactalbumin (α-La) in lactose samples. Chromatographic separation was performed on an Acquity UPLC BEH300 C18 column (2.1×150 mm, 1.7 μm) with an isocratic mobile phase consisting of water containing 0.1% TFA and acetonitrile containing 0.1% TFA (80 : 20, v/v). Mass spectrometric detection was achieved by a triple-quadrupole mass spectrometer equipped with an ESI interface operating in positive ionization mode. Quantitation was performed using selected ion monitoring ofm/z2364 forα-La. The calibration curve was linear from 0.2 to 10 µg/mL. The intra- and interday precisions were less than 7.6% and the accuracy ranged from 96.4 to 104.5%. The limit of quantification (LOQ) was 0.15 µg/mL and the limit of detection (LOD) was 0.05 µg/mL. This method was then successfully applied to investigate 6 different lactose samples. The application can provide technical preparation for the development of specification of lactose.

scholarly journals Determination of sarecycline by UPLC-MS/MS and its application to pharmacokinetic study in rats

2020 ◽  
Author(s):  
Yonghui Shen ◽  
Deru Meng ◽  
Feifei Chen ◽  
Hui Jiang ◽  
Liming Hu ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Chronic Inflammatory Disease ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Acquity Uplc ◽  
Intravenous And Oral Administration

AbstractSarecycline is a narrow-spectrum antibiotic for the treatment of acne, which is a chronic inflammatory disease of the hair follicle sebaceous glands. In the study, UPLC-MS/MS was used to establish a rapid and accurate analytical method. The sarecycline was determined with poziotinib as internal standard (IS) in rat plasma. An ACQUITY UPLC HSS T3 column (2.1 × 100 mm, 1.8 μm) could performe chromatographic separation with the mobile phase (methanol: water of 0.1% formic acid) with gradient elution. The ions of target fragment were m/z 488.19→410.14 for sarecycline and m/z 492.06→354.55 for poziotinib, which could quantify the electrospray ionization of positive multiple reaction monitoring (MRM) mode. The linear calibration curve of the concentration range was 1–1,000 ng/mL for sarecycline with a lower limit of quantification (LLOQ) of 1 ng/mL. The mean recovery was between 82.46 and 95.85% for sarecycline and poziotinib in rat plasma. RSD for precision of inter-day and intra-day were between 3.24 and 13.36%, and the accuracy ranged from 105.26 to 109.75%. The developed and validated method was perfectly used in the pharmacokinetic study and bioavailability of sarecycline after intravenous and oral administration in rats.

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