scholarly journals Quantitative determination and validation of 17 cannabinoids in cannabis and hemp using liquid chromatography-tandem mass spectrometry

2020 ◽  
Vol 412 (27) ◽  
pp. 7381-7393 ◽  
Author(s):  
Garnet McRae ◽  
Jeremy E. Melanson
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Intermediate Precision ◽  
Chromatography Tandem Mass Spectrometry ◽  
Sample Extraction ◽  
Cannabidiolic Acid ◽  
Wide Range ◽  
Liquid Chromatography Tandem Mass

Abstract The increase in production of cannabis for medical and recreational purposes in recent years has led to a corresponding increase in laboratories performing cannabinoid analysis of cannabis and hemp. We have developed and validated a quantitative liquid chromatography-tandem mass spectrometry (LC-MS/MS) method that is simple, reliable, specific, and accurate for the analysis of 17 cannabinoids in cannabis and hemp. Liquid-solid sample extraction coupled with dilution into a calibration range from 10 to 10,000 ng/mL and LC-MS/MS analysis provides quantification of samples ranging from 0.002 to 200 mg/g (0.0002 to 20.0%) in matrix. Linearity of calibration curves in methanol was demonstrated with regression r2 ≥ 0.99. Within-batch precision (0.5 to 6.5%) and accuracy (91.4 to 108.0%) and between-batch precision (0.9 to 5.1%) and accuracy (91.5 to 107.5%) were demonstrated for quality control (QC) samples in methanol. Within-batch precision (0.2 to 3.6%) and accuracy (85.4 to 111.6%) and between-batch precision (1.4 to 6.1 %) and accuracy (90.2 to 110.3%) were also evaluated with a candidate cannabis certified reference material (CRM). Repeatability (1.5 to 12.4% RSD) and intermediate precision (2.2 to 12.8% RSD) were demonstrated via analysis of seven cannabis samples with HorRat values ranging from 0.3 to 3.1. The method provides enhanced detection limits coupled with a large quantitative range for 17 cannabinoids in plant material. It is suitable for a wide range of applications including routine analysis for delta-9-tetrahydrocannabinol (Δ9-THC), delta-9-tetrahydrocannabinolic acid (Δ9-THCA), cannabidiol (CBD), cannabidiolic acid (CBDA), and cannabinol (CBN) as well as more advanced interrogation of samples for both major and minor cannabinoids.

scholarly journals Determination of Ephedra Alkaloids by Liquid Chromatography/Tandem Mass Spectrometry

2003 ◽  
Vol 86 (3) ◽  
pp. 471-475 ◽  
Author(s):  
Darryl Sullivan ◽  
James Wehrmann ◽  
John Schmitz ◽  
Richard Crowley ◽  
Jeffrey Eberhard
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Correlation Coefficients ◽  
Tandem Mass ◽  
Ephedra Sinica ◽  
Chromatography Tandem Mass Spectrometry ◽  
Wide Range ◽  
Liquid Chromatography Tandem Mass

Abstract In conjunction with an AOAC Task Group on dietary supplements, a liquid chromatography/tandem mass spectrometry (LC–MS/MS) method was validated for measurement of 6 major alkaloids in raw ephedra sinica herb, ephedra extracts, ephedra tablets, complex dietary supplements containing ephedra, and a high-protein drink mix containing ephedra. The amount of ephedrine-type alkaloids present was determined by LC with mass selective detection. Six replicates of each matrix were analyzed on 3 separate occasions. The presence of 6 ephedrine-type alkaloids was detected at a level >0.5 μg/g based on a 0.5 g sample. The standard curve range for this assay is from 0.02 to 1.0 μg/mL. Appropriate dilutions covered a wide range of specific alkaloid concentrations. The calibration curves for all 6 analytes had correlation coefficients >0.995.

scholarly journals Rapid Method for the Determination of Thiamine and Pantothenic Acid in Infant Formula and Milk-Based Nutritional Products by Liquid Chromatography‒Tandem Mass Spectrometry

2020 ◽  
Vol 103 (3) ◽  
pp. 812-817
Author(s):  
Brendon D Gill ◽  
Sheila C Saldo ◽  
Iain J McGrail ◽  
Jackie E Wood ◽  
Harvey E Indyk
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Infant Formula ◽  
Rapid Method ◽  
Pantothenic Acid ◽  
Tandem Mass ◽  
Intermediate Precision ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Abstract Background Thiamine and pantothenic acid play a critical role in numerous metabolic reactions and are typically supplemented in infant and adult nutritional formulas as thiamine chloride hydrochloride and calcium pantothenate salts. Objective A rapid compliance method for the analysis of thiamine and pantothenic acid applicable to infant formula and milk-based nutritional products is described. Method Proteins are removed by centrifugal ultrafiltration, followed by analysis by reversed-phase liquid chromatography‒tandem mass spectrometry (LC-MS/MS), with quantitation accomplished by internal standard technique. Results The method was shown to be accurate, with acceptable recovery (thiamine, 99.3–101.1%; pantothenic acid, 99.2–108.6%). A certified reference material (NIST 1849a), showed no statistical bias (α = 0.05) for thiamine (P = 0.64); although a statistically significant bias (P < 0.01) for pantothenic acid was found, the nominal bias was only 4.7% (mean = 7.1 mg/hg; certified value = 6.8 mg/hg). A comparison of results by LC-MS/MS and current methods showed negligible bias (mean bias: thiamine, 0.01 mg/hg; pantothenic acid, 0.17 mg/hg) and no statistical significance (α = 0.05; thiamine, P = 0.399; pantothenic acid, P = 0.058). Acceptable precision was demonstrated with a repeatability of 7.2% repeatability relative standard deviation (RSDr) (HorRat: 0.6) and an intermediate precision of 7.0% RSD for thiamine, and a repeatability of 5.7% RSDr (HorRat: 0.5) and an intermediate precision of 6.1% RSD for pantothenic acid. Conclusions This rapid method is intended for use in high-throughput laboratories as part of routine product compliance release testing of thiamine and pantothenic acid in manufactured infant and milk-based nutritional products.

scholarly journals Multianalyte Quantification of Vitamin B6 and B2 Species in the Nanomolar Range in Human Plasma by Liquid Chromatography–Tandem Mass Spectrometry

2005 ◽  
Vol 51 (7) ◽  
pp. 1206-1216 ◽  
Author(s):  
Øivind Midttun ◽  
Steinar Hustad ◽  
Einar Solheim ◽  
Jørn Schneede ◽  
Per M Ueland
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Cognitive Disorders ◽  
Reversed Phase ◽  
Flavin Mononucleotide ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Wide Range ◽  
Liquid Chromatography Tandem Mass

Abstract Background: Homocysteine, a risk factor of cardiovascular disease, cognitive disorders, and pregnancy complications, exists at a point of metabolic convergence of several B vitamins, including vitamins B6 and B2 (riboflavin). Measurement of the various forms of these vitamins may be useful for the study of hyperhomocysteinemia as well as for the assessment of vitamin status. Methods: Plasma (60 μL) was deproteinized by mixing with an equal volume of 50 g/L trichloroacetic acid that contained d2-pyridoxal 5′-phosphate, d3-pyridoxal, and d8-riboflavin as internal standards. Pyridoxal (PL), pyridoxal 5′-phosphate (PLP), pyridoxine (PN), pyridoxine 5′-phosphate, pyridoxamine (PM), pyridoxamine 5′-phosphate, 4-pyridoxic acid (PA), riboflavin, flavin mononucleotide (FMN), and FAD were separated on a C8 reversed-phase column, which was developed with an acetonitrile gradient in a buffer containing acetic acid and heptafluorobutyric acid. The analytes were detected by tandem mass spectrometry in the positive-ion mode. Results: The chromatographic run lasted 8 min. Within- and between-day CVs were 3%–20% and 6%–22%, respectively, and recoveries were 78%–163%. Limits of detection (signal-to-noise ratio = 5) were in the range 0.1–4.0 nmol/L, and the response was linear over several orders of magnitude. In samples from 94 healthy persons, we obtained median concentrations (nmol/L) of 35.4 for PLP, 16.9 for PL, 22.4 for PA, 10.3 for riboflavin, 7.5 for FMN, and 63.1 for FAD. PN and PM were also detected in some cardiovascular patients taking B6 supplements. Conclusions: This method based on liquid chromatography–tandem mass spectrometry measures all known plasma forms of vitamins B6 and B2, which span a wide range of polarity. The assay is characterized by simple sample processing with no derivatization, low sample volume requirement, and a short run time.

Developments in mycotoxin analysis: an update for 2011-2012

2013 ◽  
Vol 6 (1) ◽  
pp. 3-30 ◽  
Author(s):  
G.S. Shephard ◽  
F. Berthiller ◽  
P.A. Burdaspal ◽  
C. Crews ◽  
M.A. Jonker ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Ergot Alkaloids ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Wide Range ◽  
Rapid Spread ◽  
Liquid Chromatography Tandem Mass ◽  
Mycotoxin Analysis

This review highlights developments in mycotoxin analysis and sampling over a period between mid-2011 and mid- 2012. It covers the major mycotoxins aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxin, patulin, trichothecenes, and zearalenone. A section on mycotoxins in botanicals and spices is also included. Methods for mycotoxin determination continue to be developed using a wide range of analytical systems ranging from rapid immunochemical-based methods to the latest advances in mass spectrometry. This review follows the format of previous reviews in this series (i.e. sections on individual mycotoxins), but due to the rapid spread and developments in the field of multimycotoxin methods by liquid chromatography-tandem mass spectrometry, a separate section has been devoted to advances in this area of research.

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