scholarly journals Single-Run Separation and Quantification of 14 Cannabinoids Using Capillary Electrophoresis

Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 30
Author(s):  
Emil A. Zaripov ◽  
Tiah Lee ◽  
Yuchu Dou ◽  
Cory S. Harris ◽  
Artem Egorov ◽  
...  

Quantification of major cannabinoids in cannabis products is normally performed using high-pressure liquid chromatography (HPLC)-based methods. We propose a cost-effective alternative method that successfully separates and quantifies 14 cannabinoids in a single run using capillary electrophoresis (CE) coupled with a UV detector in 18 min. The separation is carried out in 60% acetonitrile in the presence of 6.5 mM sodium hydroxide and 25 µM β-cyclodextrin, resulting in good separation of cannabinoids. Our CE method demonstrated the limit of detection between 1.2–1.8 µg/mL, with the linear range reaching up to 50 µg/mL. We validated the method performance by testing a plant extract and quantifying cannabinoid content. This method is the first to separate 14 cannabinoids in one run using a CE system with UV detection.

2020 ◽  
Author(s):  
Emil Zaripov ◽  
Tiah Lee ◽  
Yuchu Dou ◽  
Cory Harris ◽  
Artem Egorov ◽  
...  

Abstract The legalization of cannabis has magnified the importance of determining the quantity and identification of cannabinoids. Both industry and consumers are highly interested in the content of cannabinoids available in their products, while health care professionals and regulators are concerned with the safety of cannabis. Quantification of major cannabinoids in products answers some of these concerns. Currently, popular methods of quantifying cannabinoids use high-pressure liquid chromatography (HPLC). Still, these HPLC methods are limited to quantifying a small number of cannabinoids unless more powerful but more costly instruments are employed to achieve better analysis, such as UHPLC and mass spectrometry. We propose a quick method that successfully separates and quantifies 14 cannabinoids in a single run using capillary electrophoresis (CE) coupled with a UV detector in 25 minutes. Our CE method demonstrated the limit of detection between 1.2–1.8 µg/mL, with the detection range reaching up to 50 µg/mL.


Author(s):  
Raju Chandra ◽  
Manisha Pant ◽  
Harchan Singh ◽  
Deepak Kumar ◽  
Ashwani Sanghi

A reliable and reproducible reversed-phase high performance liquid chromatography (RP-HPLC) was developed for the quantitative determination of Remipril drug content from marketed bulk tablets. The active ingredient of Remipril separation achieved with C18 column using the methanol water mobile phase in the ratio of 40:60 (v/v). The active ingredient of the drug content quantify with UV detector at 215 nm. The retention time of Remipril is 5.63 min. A good linearity relation (R2=0.999) was obtained between drug concentration and average peak areas. The limit of detection and limit of quantification of the instrument were calculated 0.03 and 0.09 µg/mL, respectively. The accuracy of the method validation was determined 102.72% by recoveries method.


2011 ◽  
Vol 140 ◽  
pp. 296-301 ◽  
Author(s):  
Cai Mei Wu ◽  
Hong Min Yuan ◽  
Gang Jia ◽  
Zhi Sheng Wang ◽  
Xiu Qun Wu

A reversed high performance liquid chromatography method was developed for the quantitative determination of mimosine and 2,3-DHP in leaves ofLeucaena Leucocephala. Mimosine and 2,3DHP were extracted using 0.1N HCl.The chromatograph conditions were investigated and optimized. The optimal HPLC conditions as follows: Agilent HC-C18 column (4.6×150mm,5μm) was used at 30°C. The method used a variable wavelength UV detector at 280nm, the mobile phase consisted of 0.2 % (w/v) orthophosphoric acid and methanol, the gradient elution was adopted. The injection volume was 10μL. The linearity is favorable in the range of 1.0 to 50μg mL-1with a correlation coefficient of 0.99998 for mimosine and 0.99902 for 2,3DHP. Under the optimal conditions, the method limit of detection (LOD) of mimosine and 2,3DHP were 0.40mg/kg and 0.55mg/kg respectively. The recovery of mimosine was 87.00-94.70% with the RSD (n=5) of 2.75-3.81% in the spiked levels 0,1, 5, 20mg/g. At the same time, the recovery of 2,3DHP was 88-95.4% with the RSD (n=5) of 2.24-4.90%. The method was found to be simple, sensitive, fast and accurate, and has been applied successfully for the quantitative detection of mimosine and 2,3-DHP in leaves ofLeucaena Leucocephala, plasma and excretion of ruminant.


1999 ◽  
Vol 82 (4) ◽  
pp. 809-813 ◽  
Author(s):  
Mamun M Or-Rashid ◽  
Ryoji Onodera ◽  
Shaila Wadud ◽  
Mohamed-Emad A Nasser ◽  
Mohammad R Amin

Abstract A simple, rapid, and sensitive method was developed for detection and quantitation of lysine (Lys) in various biological samples by isocratic liquid chromatography (LC). Samples containing Lys and other amino acids were derivatized with 9-fluorenylmethyl chloroformate (FMOC-CI). The mobile phase used for isocratic elution was 50 mmol/L sodium acetate buffer (pH 4.20)-acetonitrile (43 + 57, v/v). Lys was detected with a UV detector at 265 nm. The derivatized Lys eluted from a LiChrospher 100 RP-18 (150× 4.0 mm id) column at a retention time of 5.6 min. The limit of detection was 0.73 μmol/L (signal-to-noise [S/N] ratio, 3:1), and the limit of quantitation was 2.37 μmol/L (S/N ratio, 10:1). Lys recoveries from fortified biological samples were >97.5%. Average Lys contents found in rumen fluid samples collected before the morning feeding and at 2.0,4.0, and 6.0 h after feeding were 4.26,3.34,3.58, and 3.82 μmol/L, respectively. The hydrolysate of a sample of mixed rumen microorganisms collected before the morning feeding was determined to contain 1.372 μmol/mg microbial nitrogen in the form of Lys. The Lys concentrations of human plasma, goat plasma, human urine, and goat urine were 140.0, 102.0,58.0, and 32.0 μmol/L, respectively.


1979 ◽  
Vol 62 (6) ◽  
pp. 1222-1230
Author(s):  
William P Cochrane ◽  
Monique Lanouette ◽  
Roy Greenhalgh

Abstract Technical grade samples of fenitrothion were analyzed by high pressure liquid chromatography (HPLC) on a reverse phase LiChrosorb RP-8 column, using 3 solvent systems and a UV detector set at 269 nm. All commercial samples analyzed contained >94% fenitrothion; in addition, 9 contaminants were identified and quantitated. Bisfenitrothion was the major contaminant, with average amounts of 2.46% from one manufacturer and 1.17% from another. The second most abundant toxicant was S-methyl fenitrothion, which was present at an average level of 0.71% in one source but only 0.16% in the other. The amount of fenitrooxon was 0.046% or less in samples from 2 manufacturers. Other contaminants quantitated include the 2 demethyl fenitrothion isomers, 3-methyl-4-nitrophenol, 3-methyl-6-nitrophenol, 3-methyI-4-nitroanisole, and bis-S-methyl fenitrothion. The total amount of the constituents quantitated in 9 commercial samples was 99.07 ± 1.81%. By comparing the amounts of bis-fenitrothion and phenols present in technical grade fenitrothion, it should be possible to identify the specific manufacturers of the various products.


1975 ◽  
Vol 21 (12) ◽  
pp. 1774-1776 ◽  
Author(s):  
Daniel S Sitar ◽  
Kenneth M Piafsky ◽  
Robert E Rangno ◽  
Richard I Ogilvie

Abstract We present a specific, sensitive high-pressure liquidchromatographic assay for theophylline in plasma. Only 0.5 ml of plasma is required for each determination, and the lower limit of detection by this method is 0.1 mg/ liter. Other xanthines and their metabolites do not interfere. This method is suitable for use in studying the pharmacokinetics of this drug in infants and children, from whom only small volumes of blood are available.


2009 ◽  
Vol 26 (1) ◽  
pp. 19-26 ◽  
Author(s):  
Gašper Berginc ◽  
Damjan Glavač

MSI analysis is becoming increasingly important for the detection of both hereditary non-polyposis colorectal cancer and sporadic primary colorectal tumours with MSI high phenotype. The Bethesda panel of five microsatellite markers has been proposed to provide uniform criteria for MSI analysis. Here we report on an MSI analysis approach using quasimonomorphic mononucleotide repeats and denaturating high performance liquid chromatography (DHPLC). We analysed 595 newly diagnosed colorectal tumours and 145 normal samples. Microsatellite markers BAT-25, BAT-26, NR-21, NR-22, and NR-27 were amplified in multiplex reaction and analysed using DHPLC and capillary electrophoresis (CE). DHPLC conditions for analysis of MSI multiplex assay were evaluated and tested. Analysis and cross-examination of the results obtained from 96 samples using DHPLC and capillary electrophoresis showed the same sensitivity and specificity of the two approaches for detecting MSI-H tumours. Using our new approach we showed that the tested markers are quasimonomorphic in a Slovenian population, with frequencies of polymorphisms 0.07%, 1.4%, 2.1%, 1.4%, and 1.4% for BAT-25, BAT-26, NR-21, NR-22, and NR-27, respectively. Forty-three (7.2%) new MSI-H tumours were identified, of which 84% showed instability in all 5 tested markers. Overall, we developed a high-throughput, robust, accurate and cost-effective approach for the detection of MSI-H tumours.


1999 ◽  
Vol 44 (3) ◽  
pp. 14496J ◽  
Author(s):  
Richard M. Iwanicki ◽  
Kristi Maier ◽  
Joel A. Zlotnick ◽  
Ray H. Liu ◽  
Tsung-Li Kuo ◽  
...  

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