Rapid Identification of 44 Steroids in Human Urine Samples using HPLC-ESI-QTOF-MS

2021 ◽  
Vol 17 ◽  
Author(s):  
Aarti Yadav ◽  
Rajesh Dabur
Keyword(s):  
Direct Methods ◽  
High Sensitivity ◽  
Ultra Performance Liquid Chromatography ◽  
Urine Samples ◽  
Time Saving ◽  
Fast Analysis ◽  
Significant Information ◽  
Congenital Deficiency ◽  
Urinary Steroids ◽  
Tof Ms

Objective: Detailed analysis of un-processed and un-derivatized free and conjugated urinary steroids is useful to avoid miscalculations and to diagnose sports doping and adrenal problems including abnormal steroidogenesis, congenital deficiency of related enzymes, cancer, and other disease conditions. Hence, the present study was conducted to develop a soft ionization method to identify the maximum number of urinary steroids using ultra-performance liquid chromatography coupled with quadrupole time of flight mass spectrometer (HPLC–Q-TOF-MS). Material and Methods: HPLC–Q-TOF-MS was carried out for the qualitative detection of steroids and their conjugates in urine samples. The method provides high sensitivity and fast analysis of steroids and their glucuronides without hydrolysis or sample preparation or extraction of steroids. Results: Using the method, 44 steroids belonging to C-18, C-19, and C-21 classes and their conjugates were resolved and identified using positive and negative modes of ionizations by their characteristic ionization and collision energy induced dissociation behaviors. Conclusion: The method is time-saving and good to compare samples from different peoples with control or healthy ones as it doesn’t require any kind of pre-treatment or sample processing. It provides a complete picture of steroids metabolism and catabolism. It can be good for doping control or to explore the effects of other drugs. However, in qualitative analysis one may miss the significant information unless direct methods of steroids analysis to be employed.

scholarly journals A New UPLC-qTOF Approach for Elucidating Furan and 2-Methylfuran Metabolites in Human Urine Samples after Coffee Consumption

Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 5104
Author(s):  
Simone Stegmüller ◽  
Nadine Beißmann ◽  
Jonathan Isaak Kremer ◽  
Denise Mehl ◽  
Christian Baumann ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Intervention Studies ◽  
Coffee Consumption ◽  
Ultra Performance Liquid Chromatography ◽  
In Vitro Studies ◽  
Urine Samples ◽  
Tandem Mass ◽  
Time Saving ◽  
Additional Information

We have investigated urine samples after coffee consumption using targeted and untargeted approaches to identify furan and 2-methylfuran metabolites in urine samples by UPLC-qToF. The aim was to establish a fast, robust, and time-saving method involving ultra-performance liquid chromatography-quantitative time-of-flight tandem mass spectrometry (UPLC-qToF-MS/MS). The developed method detected previously reported metabolites, such as Lys-BDA, and others that had not been previously identified, or only detected in animal or in vitro studies. The developed UPLC-qToF method detected previously reported metabolites, such as lysine-cis-2-butene-1,4-dial (Lys-BDA) adducts, and others that had not been previously identified, or only detected in animal and in vitro studies. In sum, the UPLC-qToF approach provides additional information that may be valuable in future human or animal intervention studies.

Facile and Fast Detection of Genistein in Derris scandens by Square Wave Voltammetry using a Cobalt(II) Phthalocyanine-Modified Screen-Printed Electrochemical Sensor

2020 ◽  
Vol 16 (3) ◽  
pp. 341-348
Author(s):  
Surinya Traipop ◽  
Suchada Chuanuwatanakul ◽  
Orawon Chailapakul ◽  
Eakkasit Punrat
Keyword(s):  
Electrochemical Sensor ◽  
Square Wave Voltammetry ◽  
Silver Chloride ◽  
Reference Electrode ◽  
High Sensitivity ◽  
Plastic Substrate ◽  
Fast Analysis ◽  
Square Wave ◽  
Wave Voltammetry ◽  
Screen Printed

Background: Recently, Derris scandens, a Thai herbal medicine with anti-inflammatory activity, is widely used as beverage and supplementary food. When the traditional medicine is a choice for health therapy, the simple and reliable equipment is required to control the suitable consuming amount of the active component. Objective: To develop the electrochemical sensor for genistein determination in Derris scandens with high sensitivity and rapid operation. Methods: An in-house screen-printed electrochemical sensor consisting of a three-electrode system was developed for genistein determination. A silver/silver chloride (Ag/AgCl) reference electrode, a carbon counter electrode and a carbon working electrode were prepared on a 0.3-mm-thick plastic substrate by the screen-printing technique using conductive ink. The dimensions of each sensor were 2.5×1.0 cm. Only 50 µL of sample solution was required on this device for the determination of genistein concentration by rapid response square wave voltammetry. Results: The oxidation peak of genistein appeared with good response in acidic media at a peak potential of 0.6 V. Moreover, the signal was enhanced by modifying the conductive carbon ink with cobalt( II) phthalocyanine. Under the optimized conditions, the linear range was found to be 2.5-150 µM and the detection limit was 1.5 µM. Moreover, the small volume extraction was successfully developed without any further pre-concentration. This proposed method was applied to determine genistein in Derris scandens with satisfying results. Conclusion: The proposed method is promising as an alternative method for genistein determination with facile and fast analysis.

scholarly journals Diagnostic accuracy of MALDI-TOF mass spectrometry for the direct identification of clinical pathogens from urine

Open Medicine ◽  
2020 ◽  
Vol 15 (1) ◽  
pp. 266-273
Author(s):  
Min Tang ◽  
Jia Yang ◽  
Ying Li ◽  
Luhua Zhang ◽  
Ying Peng ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Likelihood Ratio ◽  
Meta Analysis ◽  
Positive Likelihood Ratio ◽  
Negative Likelihood Ratio ◽  
Urine Samples ◽  
Direct Identification ◽  
Maldi Tof Ms ◽  
Maldi Tof ◽  
Tof Ms

AbstractMatrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) has become one of the most popular methods for the rapid and cost-effective detection of clinical pathogenic microorganisms. This study aimed to evaluate and compare the diagnostic performance of MALDI-TOF MS with that of conventional approaches for the direct identification of pathogens from urine samples. A systematic review was conducted based on a literature search of relevant databases. The pooled sensitivity, specificity, positive likelihood ratio (PLR), negative likelihood ratio (NLR) and area under the summary receiver operating characteristic (SROC) curve of the combined studies were estimated. Nine studies with a total of 3920 subjects were considered eligible and included in the meta-analysis. The pooled sensitivity was 0.85 (95% CI 0.79-0.90), and the pooled specificity was 0.93 (95% CI 0.82-0.97). The PLR and NLR were 11.51 (95% CI 4.53-29.26) and 0.16 (95% CI 0.11-0.24), respectively. The area under the SROC curve was 0.93 (95% CI 0.91-0.95). Sensitivity analysis showed that the results of this meta-analysis were stable. MALDI-TOF MS could directly identify microorganisms from urine samples with high sensitivity and specificity.

scholarly journals The Double Face of Ketamine—The Possibility of Its Identification in Blood and Beverages

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 813
Author(s):  
Magdalena Świądro ◽  
Paweł Stelmaszczyk ◽  
Irena Lenart ◽  
Renata Wietecha-Posłuszny
Keyword(s):  
Date Rape ◽  
Signal To Noise Ratio ◽  
High Sensitivity ◽  
Heroin Addiction ◽  
Assisted Extraction ◽  
Low Concentrations ◽  
High Concentrations ◽  
Rosé Wine ◽  
Tof Ms

The purpose of this study was to develop and validate a high-sensitivity methodology for identifying one of the most used drugs—ketamine. Ketamine is used medicinally to treat depression, alcoholism, and heroin addiction. Moreover, ketamine is the main ingredient used in so-called “date-rape” pills (DRP). This study presents a novel methodology for the simultaneous determination of ketamine based on the Dried Blood Spot (DBS) method, in combination with capillary electrophoresis coupled with a mass spectrometer (CE-TOF-MS). Then, 6-mm circles were punched out from DBS collected on Whatman DMPK-C paper and extracted using microwave-assisted extraction (MAE). The assay was linear in the range of 25–300 ng/mL. Values of limits of detection (LOD = 6.0 ng/mL) and quantification (LOQ = 19.8 ng/mL) were determined based on the signal to noise ratio. Intra-day precision at each determined concentration level was in the range of 6.1–11.1%, and inter-day between 7.9–13.1%. The obtained precision was under 15.0% (for medium and high concentrations) and lower than 20.0% (for low concentrations), which are in accordance with acceptance criteria. Therefore, the DBS/MAE/CE-TOF-MS method was successfully checked for analysis of ketamine in matrices other than blood, i.e., rose wine and orange juice. Moreover, it is possible to identify ketamine in the presence of flunitrazepam, which is the other most popular ingredient used in DRP. Based on this information, the selectivity of the proposed methodology for identifying ketamine in the presence of other components of rape pills was checked.

scholarly journals Quantitation of Benzodiazepines and Metabolites in Urine by Liquid Chromatography–Tandem Mass Spectrometry

2018 ◽  
Vol 3 (3) ◽  
pp. 397-407
Author(s):  
Yu Zi Zheng ◽  
Dustin R Bunch ◽  
Katherine Lembright ◽  
Sihe Wang
Keyword(s):  
Precise Measurement ◽  
High Sensitivity ◽  
Urine Samples ◽  
Limit Of Quantification ◽  
Internal Standards ◽  
Independent Laboratory ◽  
Chromatography Tandem Mass Spectrometry ◽  
Analytical Recovery ◽  
Liquid Chromatography Tandem Mass ◽  
Analytical Time

Abstract Background Benzodiazepines (BZDs) are central nervous system depressants that are prescribed to prevent seizures, manage anxiety, or help sleep. When misused, BZDs can lead to addiction and sometimes cause death. Measurement of BZDs in urine is used to identify their use, especially in pain management settings. LC-MS/MS is preferred for these measurements because of its high sensitivity and specificity. Here, we report an LC-MS/MS assay for measuring 7 BZDs and metabolites in urine. Methods Urine sample was incubated at 60 °C for 30 min after addition of internal standards and a β-glucuronidase solution. After centrifugation, the supernatant was diluted with methanol and water before being injected onto a C18 analytical column in an LC-MS/MS system for quantification. The analytical time between injections was 4.35 min. The analytes included 7-aminoclonazepam, α-hydroxyalprazolam, α-hydroxytriazolam, oxazepam, lorazepam, nordiazepam, and temazepam. Results The lower limit of quantification ranged from 30 ng/mL to 50 ng/mL with an analytical recovery >80% for all 7 analytes. Total CV was <10% for all analytes (3 concentration levels of 100, 2500, and 5000 ng/mL; n = 30 each). This method had 100% agreement with a GC-MS method offered by an independent laboratory for negative urine samples. For the positive urine samples, this method showed a strong correlation (R > 0.96) with the GC-MS method. Conclusions The LC-MS/MS assay allows accurate and precise measurement of 7 BZDs and metabolites in a single analytical run with a short analytical run time and broad measuring ranges.

scholarly journals An Accurate and Effective Method for Measuring Osimertinib by UPLC-TOF-MS and Its Pharmacokinetic Study in Rats

Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2894 ◽  
Author(s):  
Song-Tao Dong ◽  
Ying Li ◽  
Hao-Tian Yang ◽  
Yin Wu ◽  
Ya-Jing Li ◽  
...  
Keyword(s):  
Matrix Effects ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Analysis Method ◽  
T790m Mutation ◽  
Flight Mass Spectrometry ◽  
Relative Standard ◽  
New Generation ◽  
Tof Ms

Osimertinib, a new-generation inhibitor of the epidermal growth factor, has been used for the clinical treatment of advanced T790M mutation-positive tumors. In this research, an original analysis method was established for the quantification of osimertinib by ultra-performance liquid chromatography with time of flight mass spectrometry (UPLC-TOF-MS) in rat plasma. After protein precipitation with acetonitrile and sorafinib (internal standard, IS), they were chromatographed through a Waters XTerra MS C18 column. The mobile phase was acetonitrile and water (including 0.1% ammonia). The relative standard deviation (RSD) of the intra- and inter-day results ranged from 5.38 to 9.76% and from 6.02 to 9.46%, respectively, and the extraction recovery and matrix effects were calculated to range from 84.31 to 96.14% and from 91.46 to 97.18%, respectively. The results illustrated that the analysis method had sufficient specificity, accuracy and precision. Meanwhile, the UPLC-TOF-MS method for osimertinib was successfully applied into the pharmacokinetics of SD rats.

An improved method for determining microbially available phosphorus in drinking water

2016 ◽  
Vol 16 (4) ◽  
pp. 1149-1158 ◽  
Author(s):  
Gang Wen ◽  
Qin Deng ◽  
Ting-Lin Huang ◽  
Jun Ma
Keyword(s):  
Drinking Water ◽  
Microbial Consortium ◽  
Incubation Temperature ◽  
Organic Phosphorus ◽  
High Sensitivity ◽  
Cell Number ◽  
Growth Potential ◽  
Utilization Efficiency ◽  
Available Phosphorus ◽  
Time Saving

Microbially available phosphorus (MAP) is the labile phosphorus that is readily assimilated by microorganisms, which is linearly correlated to bacterial re-growth in drinking water in some regions. The conventional MAP bioassay for drinking water was originally developed by Markku based on the growth potential of Pseudomonas fluorescens P17 (P17). However, the bioassay bears some demerits, such as time-consuming and labor-intensive enumeration. For convenience, an alternative method based on a similar principle was developed to assess the content of MAP in drinking water, in which natural microbial consortium was used as inoculum instead of pure culture P17, cell number was counted using flow cytometry (FCM), and cultivation at 30 °C was adopted. Natural microbial consortium is able to efficiently utilize organic phosphorus and exhibit high sensitivity since more cells are produced per μg P utilized. FCM is a rapid method to count all bacteria growing in drinking water. With incubation temperature increasing up to 30 °C, there is a shorter test period (64 h), excellent sensitivity and better utilization efficiency for organic phosphorus. The results show that the developed bioassay is sensitive, time-saving and easily operated.

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