scholarly journals Sensitive quantitative analysis of psilocin and psilocybin in hair samples from suspected users and their distribution in seized hallucinogenic mushrooms

2021 ◽  
Author(s):  
Liying Zhou ◽  
Ping Xiang ◽  
Di Wen ◽  
Baohua Shen ◽  
Xin Wang ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Mobile Phase ◽  
Matrix Effects ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Selected Reaction Monitoring ◽  
Ultra High Pressure ◽  
Hair Samples ◽  
Limit Of Quantitation ◽  
The Matrix

Abstract Purpose In this study, we developed a very sensitive method for quantitative analysis of psilocin and psilocybin in hair samples of magic mushroom consumers. Methods The analyses were performed with pretreatments of samples, followed by ultra-high pressure liquid chromatography (LC) connected to a Q-Trap type tandem mass spectrometry (MS/MS). For LC, mobile phase (A) consisted of 0.1% formic acid in water, and mobile phase (B) was acetonitrile for gradient elution using a Acquity™ UPLC HSS T3 column. For MS/MS, electrospray ionization measurements in positive selected reaction monitoring mode were used. Results The calibration curves were linear from 5 to 500 pg/mg (r > 0.99) and no selectivity problems occurred. The limit of detection was 1 pg/mg, and the lower limit of quantitation was 5 pg/mg. The ranges of the matrix effects and recovery rates were 90.4–107% and 76.0–102%, respectively. Conclusions The concentrations of psilocin in two authentic hair were 161 and 150 pg/mg, respectively, and psilocybin was not detected from both samples. This method was also used to analyze the distribution of psilocin and psilocybin in seven hallucinogenic mushrooms. To our knowledge, this is the first demonstration of psilocin concentrations in hair samples of hallucinogenic mushroom consumers, and also our method is most sensitive for quantitative analysis of psilocin and psilocybin in hair samples.

scholarly journals Pharmacokinetic Comparisons of Eight Active Components from Raw Farfarae Flos and Honey-Processed Farfarae Flos after Oral Administration in Rats by UHPLC-MS/MS Approaches

2020 ◽  
Vol 2020 ◽  
pp. 1-11
Author(s):  
Liu Yang ◽  
Hai Jiang ◽  
Xinyue Guo ◽  
Ajiao Hou ◽  
Wenjing Man ◽  
...  
Keyword(s):  
Oral Administration ◽  
Mobile Phase ◽  
Matrix Effects ◽  
Gradient Elution ◽  
Negative Ion ◽  
Selected Reaction Monitoring ◽  
Active Components ◽  
The Matrix ◽  
Acid Aqueous Solution ◽  
Negative Ion Mode

Farfarae flos (FF) is widely used for cough over thousands of years in China, but little is known about their pharmacokinetics properties. This study was aimed to establish a rapid and accurate ultraperformance liquid chromatography with triple-quadrupole tandem mass spectrometry method for compare pharmacokinetics studies of eight active compounds after oral administration between raw and honey-processed farfarae flos extracts. Optimum separation was performed on a Thermo Hypersil GOLD C18 column (100 mm × 2.1 mm, 1.9 µm particles size) with a gradient elution of acetonitrile as mobile phase A and 0.3% formic acid aqueous solution as mobile phase B. The flow rate was set as 0.3 mL/min and separated for 34.0 minutes. Electrospray ionization in the negative ion mode and selected reaction monitoring were used to identify and separate active components. The results met the acceptance criteria and showed that this method exhibited good linear, precision, accuracy, and stability. The extraction recoveries ranged from 81.54% to 104.48%, and the matrix effects ranged from 81.94% to 103.02%. These results show that the validated method could be successfully applied to evaluate the pharmacokinetic study in rats after oral administration of raw farfarae flos (R-FF) and honey-processed farfarae flos (H-FF).

Determination of ketamine and norketamine in hair and evaluation of polydrug use in ketamine abusers using hair analysis in Korea

2020 ◽  
Author(s):  
Jongsook Rhee ◽  
Jihyun Kim ◽  
Moonhee Jang ◽  
Ilchung Shi ◽  
Sangki Lee
Keyword(s):  
Mass Spectrometry ◽  
Matrix Effects ◽  
Limit Of Detection ◽  
Gas Chromatography Mass Spectrometry ◽  
Controlled Drugs ◽  
Hair Samples ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Forensic Service

Abstract This study evaluated hair samples from 28 subjects who had measurable ketamine levels among the samples requested from 2016 to 2017 into Seoul Institute National Forensic Service in Korea. Ketamine in the hair was extracted by using a solution of 1% hydrochloric acid in methanol for 16 h. Extracts were analyzed using gas chromatography mass spectrometry (GC-MS) or liquid chromatography tandem mass spectrometry (LC-MS-MS). LC-MS-MS method was validated by determining the limit of detection (LOD), limit of quantitation (LOQ), linearity, intra- and inter-accuracy, precision, and matrix effects. In 59 ketamine-positive hair or hair segments from 28 ketamine abusers, the ketamine concentration was found to be in the range of 0.011-335.8 ng/mg (mean, 13.6; median, 1.8), and the norketamine concentration was found to be in the range of 0.001-35.7 ng/mg (mean, 7.5; median, 0.44). The ratio of norketamine to ketamine concentration in hair was in the range of 0.01-1.46 (mean, 0.34; median, 0.26). The distribution of ketamine concentration in hair samples was as follows: 0.01-0.1 ng/mg in 11 samples (18.6%), 0.1-5 ng/mg in 33 samples (55.9%), 5-10 ng/mg in 4 samples (6.8%), 10-15 ng/mg in 2 samples (3.4%), 15-20 ng/mg in 4 samples (6.8%), 40-45 ng/mg in 2 samples (3.4%), 45-50 ng/mg in 1 samples 1.7%) and >100 ng/mg in only 2 samples (3.4%). In the hair of ketamine-abusers, 26 of 28 subjects had simultaneously ketamine with detectable levels of other controlled drugs, including MDMA (n=9), MA (n=3), MDMA/MA (n=3), MDMA/PMA (n=3), MDMA/PMA/MA (n=2), cocaine (n=1), and other drugs (n=5, propofol, zolpidem or benzodiazepines). In most of the hair samples were detected ketamine with other controlled drugs: MDMA (60.7%), MA (28.6%), PMA(17.9%), zolpidem (17.9%), and propofol (14.3%) in the frequency of abuse. In conclusion, most of the ketamine-abusers (92.9%) would be polydrug abusers, who were concomitantly abusing other controlled substances.

scholarly journals Method Development and Validation for Ultra-High Pressure Liquid Chromatography/Tandem Mass Spectrometry Determination of Multiple Prostanoids in Biological Samples

2013 ◽  
Vol 96 (1) ◽  
pp. 67-76 ◽  
Author(s):  
Rui Yu ◽  
Guiqing Zhao ◽  
John W Christman ◽  
Lei Xiao ◽  
Richard B van Breemen
Keyword(s):  
High Pressure ◽  
Method Development ◽  
Matrix Effects ◽  
Selected Reaction Monitoring ◽  
Calibration Model ◽  
Ultra High Pressure ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Electrospray Ionization ◽  
Development And Validation

Abstract Following oxygenation of arachidonic acid by cyclooxygenase to form prostaglandin H2 (PGH2), a variety of prostanoids can be generated with diverse physiologic effects on pain, inflammation, allergy, cardiovascular system, cancer, etc. To facilitate the quantitative analysis of prostanoids in human serum of cell culture, an ultra-high pressure LC (UHPLC)/MS/MS method was developed and validated for the measurement of six eicosanoids belonging to the cyclooxygenase pathway: PGE2, PGD2, 8-iso-PGF2α, PGF2α, 6-keto-PGF1α, and thromboxane B2 (TXB2 ). Selectivity, matrix effects, calibration model, precision, and accuracy (intraday and interday), lower limit of quantitation (LLOQ), recovery, stability, and sample dilution were evaluated. Fast UHPLC separation was carried out in only 0.5 min with isocratic elution, and each prostanoid was measured using negative electrospray ionization MS with collision-induced dissociation and selected reaction monitoring. UHPLC/MS/MS provided high throughput with peak widths of approximately 3 s and an LLOQ of 0.020 ng/mL for PGE2, 0.027 ng/mL for PGD2, 0.152 ng/mL for 8-iso-PGF2α, 0.179 ng/mL for PGF2α and 6-keto-PGF1α, and 0.013 ng/mL for TXB2.

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

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 Fast and Validated HPLC Method for Simultaneous Determination of Dopamine, Dobutamine, Phentolamine, Furosemide, and Aminophylline in Infusion Samples and Injection Formulations

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Fuchao Chen ◽  
Baoxia Fang ◽  
Sicen Wang
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Stability Study ◽  
Precision Data ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
The Stability

A simple, fast, and validated HPLC method was developed for the simultaneous quantization of five cardiovascular agents: dopamine (DPM), dobutamine (DBM), phentolamine (PTM), furosemide (FSM), and aminophylline (APL) either in infusion samples or in an injection dosage form. The proposed method was achieved with a 150 mm × 4.6 mm, 5.0 μm C18 column, by using a simple linear gradient. Mobile phase A was buffer (50 mM KH2PO4) and mobile Phase B was acetonitrile at a flow rate of 1.0 mL/min. The column temperature was kept at 30°C, and the injection volume was 20 μL. All analytes were separated simultaneously at a retention time (tr) of 3.93, 5.84, 7.06, 8.76, and 9.67 min for DPM, DBM, PTM, FSM, and APL, respectively, with a total run time of less than 15.0 min. The proposed method was validated according to ICH guidelines with respect to accuracy, precision, linearity, limit of detection, limit of quantitation, and robustness. Linearity was obtained over a concentration range of 12.0–240.0, 12.0–240.0, 20.0–200.0, 6.0–240.0, and 10.0–200.0 μg/mL DPM, DBM, PTM, FSM, and APL, respectively. Interday and intraday accuracy and precision data were recorded in the acceptable limits. The new method has successfully been applied for quantification of all five drugs in their injection dosage form, infusion samples, and for evaluation of the stability of investigated drugs in mixtures for endovenous use. The results of the stability study showed that mixtures of DPM, DBM, PTM, FSM, and APL in 5% glucose or 0.9% sodium chloride injection were stable for 48 hours when stored in polypropylene syringes at 25°C.

scholarly journals Validated HPTLC Method for Quantification of Luteolin and Apigenin inPremna mucronataRoxb., Verbenaceae

2015 ◽  
Vol 2015 ◽  
pp. 1-7 ◽  
Author(s):  
Nayan G. Patel ◽  
Kalpana G. Patel ◽  
Kirti V. Patel ◽  
Tejal R. Gandhi
Keyword(s):  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Method ◽  
Methanolic Extract ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Reflection Mode ◽  
Limit Of Quantitation ◽  
Hptlc Method

A simple, rapid, and precise high-performance thin-layer chromatographic method was developed for quantitative estimation of luteolin and apigenin inPremna mucronataRoxb., family Verbenaceae. Separation was performed on silica gel 60 F254HPTLC plates using toluene : ethyl acetate : formic acid (6 : 4 : 0.3) as mobile phase for elution of markers from extract. The determination was carried out in fluorescence mode using densitometric absorbance-reflection mode at 366 nm for both luteolin and apigenin. The methanolic extract ofPremna mucronatawas found to contain 10.2 mg/g % luteolin and 0.165 mg/g % of apigenin. The method was validated in terms of linearity, LOD and LOQ, accuracy, precision, and specificity. The calibration curve was found to be linear between 200 and 1000 ng/band for luteolin and 50 and 250 ng/band for apigenin. For luteolin and apigenin, the limit of detection was found to be 42.6 ng/band and 7.97 ng/band while the limit of quantitation was found to be 129.08 ng/band and 24.155 ng/band, respectively. This developed validated method is capable of quantifying and resolving luteolin and apigenin and can be applicable for routine analysis of extract and plant as a whole.

Identification of Suvorexant in Blood Using LC–MS-MS: Important Considerations for Matrix Effects and Quantitative Interferences in Targeted Assays

2019 ◽  
Vol 44 (3) ◽  
pp. 245-255 ◽  
Author(s):  
Britni Skillman ◽  
Sarah Kerrigan
Keyword(s):  
Matrix Effects ◽  
Limit Of Detection ◽  
Chemical Properties ◽  
Internal Standard ◽  
Forensic Toxicology ◽  
Calibration Model ◽  
Physico Chemical ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Electrospray Interface

Abstract Suvorexant (Belsomra®) is a novel dual orexin receptor antagonist used for the treatment of insomnia. The prevalence of suvorexant in forensic samples is relatively unknown, which demonstrates the need for robust analytical assays for the detection of this sedative hypnotic in forensic toxicology laboratories. In this study, suvorexant was isolated from whole blood using a simple acidic/neutral liquid–liquid extraction followed by analysis by liquid chromatography tandem mass spectrometry (LC–MS/MS). Matrix effects were evaluated qualitatively and quantitatively using various extraction solvents, proprietary lipid clean-up devices and source conditions. The method was validated in terms of limit of detection, limit of quantitation, precision, bias, calibration model, carryover, matrix effects and drug interferences. Electrospray is a competitive ionization process whereby compounds in the droplet compete for a limited number of charged sites at the surface. As such, it is capacity-limited, and LC–MS-based techniques must be carefully evaluated to ensure that matrix effects or coeluting drugs do not impact quantitative assay performance. In this report, we describe efforts to ameliorate such effects in the absence of an isotopically labeled internal standard. Matrix effects are highly variable and heavily dependent on the physico-chemical properties of the substance. Although there is no universal solution to their resolution, conditions at the electrospray interface can mitigate these issues. Using this approach, the LC–MS/MS assay was fully validated and limits of detection and quantitation of 0.1 and 0.5 ng/mL suvorexant were achieved in blood.

Development and validation of a HPLC-UV method for the simultaneous detection and quantification of paclitaxel and sulforaphane in lipid based self-microemulsifying formulation

2019 ◽  
Vol 57 (10) ◽  
pp. 931-938 ◽  
Author(s):  
Mohammad M Kamal ◽  
Sami Nazzal
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Simultaneous Detection ◽  
Reversed Phase ◽  
Limit Of Quantitation ◽  
Development And Validation ◽  
Simultaneous Delivery ◽  
Detection And Quantification

Abstract Paclitaxel (PTX) and sulforaphane (SFN) are known anticancer molecules. Their activity was found to be potentiated when tested concurrently. Only recently, however, a novel SFN enabled PTX self-microemulsifying formulation (SMEDDS) was developed for their simultaneous delivery. This necessitated the development of an analytical method for the simultaneous detection and quantitation of PTX and SFN. In this study, a simple and sensitive isocratic high performance liquid chromatography-ultraviolet (HPLC-UV) analytical method was developed and validated per International Conference on Harmonization guidelines to satisfy this objective. Its application was demonstrated when quantifying the amount of PTX and SFN released from the SMEDDS in various dissolution media. The separation of the analytes was performed with the aid of a reversed phase C18 column at ambient temperature using a 60:40 mixture of acetonitrile and KH2PO4 buffer (pH 5.0) as the mobile phase. PTX and SFN peaks were detected at 202 nm with high resolution without interference from excipients. This method showed linearity within 2.5–100 μg/mL range with r2 > 0.999. The limit of detection and lower limit of quantitation were 0.1638 and 0.4964 μg/mL for PTX and 0.4419 and 1.3389 μg/mL for SFN, respectively. A total of 98–101% of the injected samples was recovered with RSD of 0.06–0.68% indicating the suitability of the method for the simultaneous detection and quantitation of the molecules in dissolution media.

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