Simultaneous Quantitation of Seven Phenethylamine-Type Drugs in Forensic Blood and Urine Samples by UHPLC–MS-MS

2021 ◽  
Author(s):  
Chu-An Yang ◽  
Hsiu-Chuan Liu ◽  
Ray H Liu ◽  
Dong-Liang Lin ◽  
Shu-Pao Wu
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Analytical Data ◽  
Tandem Mass ◽  
Limit Of Quantitation ◽  
Routine Identification ◽  
Urine Specimens

Abstract Abuse of new psychoactive substances (NPS) has become a health and social issue of global concern. p-Methoxyamphetamine (PMA)/p-methoxymethamphetamine (PMMA) with fluoro- or chloro-derivatives of amphetamine and methamphetamine were among the most common drugs found in specimens from fatal cases in Taiwan during the January 2011 to December 2018 period. A liquid–liquid extraction sample preparation protocol with highly sensitive ultra-high performance liquid chromatography–tandem mass spectrometry approach was developed for the simultaneous analysis of seven phenethylamine-type drugs—PMA, PMMA, p-methoxyethylamphetamine, 4-fluoroamphetamine (4-FA), 4-fluoromethamphetamine (4-FMA), 4-chloroamphetamine (4-CA) and 4-chloromethamphetamine (4-CMA)—in postmortem blood and urine specimens. Separation by liquid chromatography was performed by Agilent Zorbax SB-Aq column. Tandem mass spectrometry was operated in Agilent Jet Stream Technology electrospray ionization in positive-ion multiple reaction monitoring mode. An analytical methodology was evaluated using drug-free blood and urine after fortification with 100–2,000 ng/mL of the seven target analytes. Average extraction recoveries were >80%; slightly higher ion suppression was observed for PMA and 4-CA; intra-/inter-day precision (% coefficient of variation) and accuracy were in the ranges of 0.52–12.3% and 85–110%, respectively. Limit of detection and lower limit of quantitation for these seven analytes were both in the 0.5–5 ng/mL range. Interference and carryover were not significant. This relatively simple methodology was found effective and reliable for routine identification and quantitation of these seven analytes in postmortem and antemortem blood and urine specimens received in 2018. Analytical data obtained from these actual cases indicated the following: (i) compared to findings reported during the 2007–2011 period, the use of substituted phenethylamine-type drugs decreased in 2018; (ii) ketamine and 7-aminonimetazepam (the main metabolite of nimetazepam) were the most common co-ingested substances in specimens containing PMA/PMMA, 4-FA/4-FMA, or 4-CA/4-CMA; and (iii) in drug fatalities, the concentration of PMA was significantly higher than the concentration of PMMA in both urine and blood, while the reverse was true in urine specimens from antemortem cases.

scholarly journals Rapid detection of dimethyl yellow dye in curry by liquid chromatography-electrospray-tandem mass spectrometry

2010 ◽  
Vol 28 (No. 5) ◽  
pp. 427-432 ◽  
Author(s):  
F. Tateo ◽  
M. Bononi ◽  
F. Gallone
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Mass Spectral ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
High Degree ◽  
Positive Ion

An accurate and rapid method, was devised for the identification and quantitation of dimethyl yellow dye in curry, based on liquid chromatography-tandem mass spectrometry interfaced with electrospray. Mass spectral acquisition was done in positive ion mode applying two fragmentation transitions to provide a high degree of selectivity. The extraction system provided a very high recovery (100.0% to 105.8%) and good results were obtained for the limit of detection (5 μg/kg) and limit of quantitation (16 μg/kg). The applicability of the method to identifing and quantifing the unauthorised dimethyl yellow dye in curry was demonstrated.

scholarly journals Determination of Cyclamate in Foods by Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry

2008 ◽  
Vol 91 (5) ◽  
pp. 1095-1102 ◽  
Author(s):  
Robert Sheridan ◽  
Thomas King
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract A highly sensitive and selective method that requires minimal sample preparation was developed for the confirmation and quantitation of cyclamate in a variety of foods by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Sample preparation consisted of homogenization followed by extraction and dilution of cyclamate with water. HPLC separation was achieved using a bridged ethyl hybrid C18 high-pressure column with a mobile phase consisting of 0.15 acetic acid and methanol. Under electrospray ionization negative conditions, quantitation was achieved by monitoring the fragment m/z 79.7 while also collecting parent ion m/z 177.9. Two food matrixes, diet soda and jelly, were subjected to a validation procedure in order to evaluate the applicability of the method. The cyclamate limit of detection for both matrixes was determined to be 0.050 g/g with a limit of quantitation of 0.150 g/g. The correlation coefficient of the calibration curves was >0.9998 from 0.0005 to 0.100 g/mL. The method has been used for the determination of cyclamate in several foods and the results are presented.

scholarly journals Detection and Identification of Zeranol in Chicken or Rabbit Liver by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

2002 ◽  
Vol 85 (4) ◽  
pp. 841-847 ◽  
Author(s):  
Xiaoming Fang ◽  
Jiahua Chen ◽  
Dehua Guo ◽  
Guoquan Wang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Rabbit Liver ◽  
Negative Ion ◽  
Tandem Mass ◽  
Detection And Identification ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A sensitive, specific, and reliable liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for detection and identification of zeranol in chicken or rabbit liver. A homogenized liver sample was hydrolyzed with β-glucuronidase/arylsulfatase, and the hydrolysate was extracted with ethyl ether. The supernatant was evaporated to dryness, and the residue was dissolved in chloroform and re-extracted with sodium hydroxide. After acidification, the extract was cleaned up on a C18 solid-phase extraction cartridge and analyzed by electrospray LC-MS/MS in the negative ion mode. The multiple reaction monitoring transition from both m/z 321 to 277 and m/z 321 to 303 was monitored for confirmation, and the product ion of 277 was used for quantitation. Separation was performed on a Waters XTettra™ C18 column (50 × 2.1 mm, 3.5 μm) combined with a safeguard column (Symmetry C18, 20 × 3.9 mm, 5 μm), using a gradient elution with acetonitrile and 20mM ammonium acetate. Calibration curves were prepared and good linearity was achieved over the concentration ranges tested. For all liver samples fortified at 3 different levels of 1, 5, and 50 μg/kg, the overall recoveries and relative standard deviations were in the range of 61–90 and 8–13%, respectively. The limit of quantitation based on the assay validation was 1 μg/kg. The method had been used on a routine basis for detection and identification of zeranol in liver samples.

scholarly journals Evaluation of a rapid micro-scale assay for tacrolimus by liquid chromatography-tandem mass spectrometry

2002 ◽  
Vol 39 (5) ◽  
pp. 487-492 ◽  
Author(s):  
BG Keevil ◽  
SJ McCann ◽  
DP Cooper ◽  
MR Morris
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Immunosuppressive Drug ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Background: The immunosuppressive drug tacrolimus has complex and unpredictable pharmacokinetics, therefore regular monitoring is required in patients receiving tacrolimus therapy. We have developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for measuring tacrolimus concentrations in whole blood and have compared it with a microparticle enzyme immunoassay. Methods: For the LC-MS/MS assay, samples were prepared in a 96-deep well microtitre plate by adding 10 µL of blood to 40 µL of 0·1 mol/L zinc sulphate solution. Proteins were precipitated by adding 100 µL acetonitrile containing ascomycin internal standard. After vigorous mixing and centrifugation, 20 µL of the supernatant was injected into the LC-MS/MS system. A C18 cartridge (3 mm × 4 mm) was eluted with a step gradient of 50% to 100% methanol containing 2 mmol/L ammonium acetate and 0·1% (v/v) formic acid, at 0·6 mL/min. The column was maintained at 55°C. Results: The retention times were 0·98 min for ascomycin and 0·98 min for tacrolimus. Cycle time was 2·5 min, injection to injection. The analytes were monitored using a Quattro micro tandem mass spectrometer operated in multiple reaction monitoring mode using the following transitions: m/z821 > 768 (tacrolimus) and m/z809 > 756 (ascomycin). The limit of quantitation was 0·5 µg/L and the assay was linear up to 30 µg/L. Precision of the method, over the concentration range 2·5-15·0 µg/L, was < 7% within-batch and < 6% between-batch. Total time to analyse 24 samples including result generation was 90 min. Conclusion: We conclude that the LC-MS/MS method is quick, precise and robust and will provide a fast turn around of results for the transplant physician.

scholarly journals Application of a Reliable LC-MS/MS Method for Determination of Rizatriptan in Healthy Subject Samples: Demonstration of Assay Reproducibility by Incurred Sample Reanalysis

2012 ◽  
Vol 2012 ◽  
pp. 1-10 ◽  
Author(s):  
Dinesh S. Patel ◽  
Naveen Sharma ◽  
Mukesh C. Patel ◽  
Bhavin N. Patel ◽  
Pranav S. Shrivastav ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Quality Control ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantitation

A reliable, rapid, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay has been proposed for the determination of rizatriptan in human plasma using sumatriptan as internal standard (IS). The analyte and IS were extracted from 300 μL human plasma via liquid-liquid extraction and the chromatography was achieved on Hypurity C18 (50 mm × 4.6 mm, 5 μm) column under isocratic conditions. Detection of rizatriptan and IS was done by tandem mass spectrometry, operating in positive ionization and multiple-reaction monitoring mode. The limit of detection and lower limit of quantitation of the method were 0.04 and 0.20 ng/mL, respectively, with a linear dynamic range of 0.20–60.0 ng/mL. The intrabatch and interbatch precision (% CV) was ≤8.4% while the mean extraction recovery was >78% across quality control levels. Bench top stability, freeze and thaw stability, processed sample stability, and long-term stability in plasma were evaluated at two quality control levels. It was successfully applied to a bioequivalence study of 10 mg rizatriptan orally disintegrating tablet formulation in 40 and 32 healthy Indian male subjects under fasting and fed conditions, respectively. The reproducibility in the measurement of study data was demonstrated by reanalysis of 254 incurred samples.

scholarly journals Simultaneous determination of multi – component mycotoxin in feeds by liquid chromatography – tandem mass spectrometry

2013 ◽  
Vol 57 (4) ◽  
pp. 567-572 ◽  
Author(s):  
Katarzyna Pietruszka ◽  
Bartosz Sell ◽  
Olga Burek ◽  
Henryka Wiśniewska-Dmytrow
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Ion Trap ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
Tandem Mass ◽  
Penicillium Species ◽  
Liquid Chromatography Tandem Mass

Abstract A multiresidue method for determination and quantification of Fusarium mycotoxins: deoxynivalenol, zearalenone, T-2 toxin, HT-2 toxin, and metabolite of Aspergillus and Penicillium species - ochratoxin A in feeds was described. The method was based on the simultaneous extraction of selected mycotoxins from matrix, followed by liquid chromatography coupled with tandem mass spectrometry using a hybrid triple quadrupole - linear ion trap mass spectrometer with the multiple reaction monitoring in both positive- and negative-ion modes. The method was validated in accordance with the Commision Decision 2002/657/EC requirements. The mean recoveries of mycotoxins from spiked feed samples ranged from 74.6% to 113.9%, whereas limit of detection and quantification ranged from 0.72 to 12.4 μg/kg and 1.86 to 31.7 μg/kg, respectively.

scholarly journals Rapid Determination of Fosetyl-Aluminum Residues in Lettuce by Liquid Chromatography/Electrospray Tandem Mass Spectrometry

2003 ◽  
Vol 86 (4) ◽  
pp. 832-838 ◽  
Author(s):  
Félix Hernández ◽  
Juan V Sancho ◽  
Óscar J Pozo ◽  
Carme Villaplana ◽  
María Ibáñez ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Tandem Mass ◽  
Electrospray Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract This paper describes a new method for the sensitive and selective determination of fosetyl-aluminum (Al) residues in vegetable samples. The method involves extraction with water by using a high-speed blender and subsequent injection of the 5-fold diluted extract into the liquid chromatograph. Fosetyl-Al is determined by liquid chromatography with electrospray tandem mass spectrometry after the addition of tetrabutylammonium acetate as the ion-pairing re-agent. The method has been used to assay lettuce samples spiked at 2 and 0.2 mg/kg. Recoveries were satisfactory, with mean values of 98 and 106%, respectively, and relative standard deviations were &lt;10%. The limit of quantitation was 0.2 mg/kg, and the limit of detection was as low as 0.05 mg/kg. Matrix-matched calibration was used for quantitation, and the addition of an internal standard improved repeatability. The developed method allows the accurate and rapid determination of low levels of fosetyl-Al residues in lettuce with very little sample handling and good sensitivity; it was shown to be robust by the analysis of almost 100 samples.

scholarly journals Targeted Metabolomic Profiling of Total Fatty Acids in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry

Metabolites ◽  
2020 ◽  
Vol 10 (10) ◽  
pp. 400
Author(s):  
Anas Al Aidaros ◽  
Charu Sharma ◽  
Claus-Dieter Langhans ◽  
Jürgen G. Okun ◽  
Georg F. Hoffmann ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Fatty Acids ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Disease Risk ◽  
Multiple Reaction Monitoring ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

This article reports a targeted metabolomic method for total plasma fatty acids (FAs) of clinical or nutritional relevance. Thirty-six saturated, unsaturated, or branched-chain FAs with a chain length of C8-C28 were quantified using reversed-phase liquid chromatography-tandem mass spectrometry. FAs in plasma (10 μL) were acid-hydrolyzed, extracted, and derivatized with DAABD-AE (4-[2-(N,N-Dimethylamino)ethylaminosulfonyl]-7-(2-aminoethylamino)-2,1,3-benzoxadiazole) at 60 °C for 1 h. Derivatization resulted in a staggering nine orders of magnitude higher sensitivity compared to underivatized analytes. FAs were measured by multiple-reaction monitoring using stable isotope internal standards. With physiological and pathological analyte levels in mind, linearity was established using spiked plasma. Intra-day (n = 15) and inter-day (n = 20) imprecisions expressed as variation coefficient were ≤10.2% with recovery ranging between 94.5–106.4%. Limits of detection and limit of quantitation ranged between 4.2–14.0 and 15.1–51.3 pmol per injection, respectively. Age-stratified reference intervals were established in four categories: <1 month, 1–12 month, 1–18 year, and >18 year. This method was assessed using samples from patients with disorders affecting FAs metabolism. For the first time, C28:0 and C28:0/C22:0 ratio were evaluated as novel disease biomarkers. This method can potentially be utilized in diagnosing patients with inborn errors of metabolism, chronic disease risk estimation, or nutritional applications.

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