scholarly journals Determination of the Appetite Suppressant P57 in Hoodia gordonii Plant Extracts and Dietary Supplements by Liquid Chromatography/Electrospray Ionization Mass Spectrometry (LC-MSD-TOF) and LC-UV Methods

2006 ◽  
Vol 89 (3) ◽  
pp. 606-611 ◽  
Author(s):  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Rahul S Pawar ◽  
Yatin J Shukla ◽  
Brian Schaneberg ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Reversed Phase ◽  
Ionization Mass ◽  
Active Constituent ◽  
Appetite Suppressant ◽  
Hoodia Gordonii ◽  
Relative Standard

Abstract Hoodia gordonii is traditionally used in South Africa for its appetite suppressant properties. P57AS3 (P57), an oxypregnane steroidal glycoside, is the only reported active constituent from this plant as an appetite suppressant. Effective quality control of these extracts or products requires rapid methods to determine P57 content. New methods of liquid chromatography/mass spectrometry (LC/MS) and LC-UV for analysis of P57 from H. gordonii have been developed. The quantitative determination of P57 was achieved with a Phenomenex Gemini (Torrance, CA) reversed-phase column using gradient mobile phase of water and acetonitrile, both containing 0.1% acetic acid. The method was validated for linearity, repeatability, and limits of detection and quantification. Good results were obtained in terms of repeatability (relative standard deviation <5.0%) and recovery (98.5103.5%). The developed methods were applied to the determination of P57 for H. gordonii plant samples, one related genus (Opuntia ficus-indica), and dietary supplements that claim to contain H. gordonii.

scholarly journals Determination of 7B3 Residues in Cotton Plants by Liquid Chromatography/Mass Spectrometry

2009 ◽  
Vol 92 (1) ◽  
pp. 302-306 ◽  
Author(s):  
Xiao-Jing Yan ◽  
Xiao-Mei Liang ◽  
Yan-Jun Xu ◽  
Shu-Hui Jin ◽  
Dao-Quan Wang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Cotton Plants

Abstract A method was developed for the determination of 7B3 (12-propyloxyimino-1,15-pentadecanlactam), a novel macrolactam fungicide, by liquid chromatography/mass spectrometry (LC/MS) with positive electrospray ionization (ESI+). The method used a reversed-phase C18 column and acetonitrilewater (60 + 40, v/v) mobile phase. The quick, easy, cheap, effective, rugged, and safe method was used for extraction of 7B3 from cotton plants, which involved the extraction of 10 g homogenized sample with 10 mL acetonitrile, followed by the addition of 4 g anhydrous MgSO4 and 1.0 g NaCl. After centrifugation, 1 mL of the buffered acetonitrile extract was transferred into a tube containing 50 mg primary secondary amine sorbent and 100 mg anhydrous MgSO4. After shaking and centrifugation, the final extract was transferred to an autosampler vial for concurrent analysis by LC/MS. The results of 7B3 determined by LC/MS in the selective ion monitoring mode were linear, and the matrix effect of the method was evaluated. The average recoveries of 7B3 fortified at different levels were within 84.1100.2, and the relative standard deviations were <7.5 for all samples analyzed. The method limit of detection and the limit of quantitation values were 0.03 and 0.1 mg/kg, respectively. The proposed method was successfully applied to determine 7B3 residues in practical samples. This method is sensitive, accurate, reliable, simple, and safe.

scholarly journals Determination of Imidacloprid and Benzimidazole Residues in Fruits and Vegetables by Liquid Chromatography–Mass Spectrometry after Ethyl Acetate Multiresidue Extraction

2000 ◽  
Vol 83 (3) ◽  
pp. 748-755 ◽  
Author(s):  
Amadeo R Fernández-Alba ◽  
Ana Tejedor ◽  
Ana Agüera ◽  
Mariano Contreras ◽  
Juan Garrido
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Fruits And Vegetables ◽  
Monitoring Program ◽  
Reversed Phase ◽  
Food Samples ◽  
Ionization Mass ◽  
Vegetables And Fruits

Abstract A simple and sensitive method based on liquid chromatography–atmospheric pressure ionization–mass spectrometry is described for the determination of 4 benzimidazole pesticides (carbendazim, thiabendazole, benomyl, and thiophanate-methyl) and imidacloprid in vegetables and fruits. Food samples were typically extracted with ethyl acetate to draw the analytes into the organic phase. No cleanup step was necessary before injection into the liquid chromatographic (LC) system with electrospray mass spectrometric detection. The analytes were separated on a reversed-phase C8LC column. Limits of detection for the compounds were in the μg/L range. Results are reported for validation studies with fortified pear and tomato samples and for residues of the target compounds found in the pesticide residue monitoring program during 1998.

scholarly journals Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4399
Author(s):  
Dasom Shin ◽  
Hui-Seung Kang ◽  
Hyungsoo Kim ◽  
Guiim Moon
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

scholarly journals Simultaneous determination of seven glucocorticoids in cosmetics by liquid chromatography tandem mass spectrometry

2020 ◽  
Vol 3 (2) ◽  
pp. 115-124
Author(s):  
Dong Bui Quang ◽  
Phuong Vu Thi ◽  
Van Anh Tran Thi ◽  
Son Tran Cao ◽  
◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Fluocinolone Acetonide ◽  
Tandem Mass ◽  
Chromatography Method ◽  
Relative Standard

A rapid high-performance liquid chromatography method with electrospray ionization and tandem mass spectrometry detection (LC-ESI-MS/MS) was developed and validated for the simultaneous determination of 7 glucocorticoids (GC) including hydrocortisone acetate (HCA), cortisone acetate (COA), prednisone (PDS), prednisolone (PDL), methyl prednisolone (MPL), dexamethasone (DEX) and fluocinolone acetonide (FLA), which may be illegally blended in transdermal cosmetics. Sample preparation step consists of the extraction with ethyl acetate followed by centrifugation and filtration. The extract was dried, diluted and cleaned using C18 SPE column. The compounds were separated by reversed-phase chromatography with mobile phase containing 0.1% formic acid in water and acetonitrile in gradient condition. The method was validated at the validation level from 0.12 to 6.0 µg/g. The LODs for PDS, PDL and FLA were 0.3 µg/g and for the others were 0.03 µg/g, and LOQs were 0.6 and 0.12 µg/g, respectively. The reproducibility was satisfied with the relative standard deviation below 23% and the recoveries were in the range of 74.3-106.7% meeting AOAC requirements. The studied glucocorticoids were detected in about 20% of tested samples collected in Hanoi with the level contents in the range from 0.18 to 16.2 µg/g.

scholarly journals Determination of Aristolochic Acid in Botanicals and Dietary Supplements by Liquid Chromatography with Ultraviolet Detection and by Liquid Chromatography/Mass Spectrometry: Single Laboratory Validation Confirmation

2006 ◽  
Vol 89 (4) ◽  
pp. 942-959 ◽  
Author(s):  
William A Trujillo ◽  
Wendy R Sorenson ◽  
Paul La Luzerne ◽  
John W Austad ◽  
Darryl Sullivan
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Aristolochic Acid ◽  
Automation System ◽  
Ultraviolet Detection ◽  
Relative Standard ◽  
Single Laboratory ◽  
Aristolochic Acid I

Abstract The presence of aristolochic acid in some dietary supplements is a concern to regulators and consumers. A method has been developed, by initially using a reference method as a guide, during single laboratory validation (SLV) for the determination of aristolochic acid I, also known as aristolochic acid A, in botanical species and dietary supplements at concentrations of approximately 2 to 32 μg/g. Higher levels were determined by dilution to fit the standard curve. Through the SLV, the method was optimized for quantification by liquid chromatography with ultraviolet detection (LC-UV) and LC/mass spectrometry (MS) confirmation. The test samples were extracted with organic solvent and water, then injected on a reverse phase LC column. Quantification was achieved with linear regression using a laboratory automation system. The SLV study included systematically optimizing the LC-UV method with regard to test sample size, fine grinding of solids, and solvent extraction efficiency. These parameters were varied in increments (and in separate optimization studies), in order to ensure that each parameter was individually studied; the test results include corresponding tables of parameter variations. In addition, the chromatographic conditions were optimized with respect to injection volume and detection wavelength. Precision studies produced overall relative standard deviation values from 2.44 up to 8.26% for aristolochic acid I. Mean recoveries were between 100 and 103% at the 2 μg/g level, between 102 and 103% at the 10 μg/g level, and 104% at the 30 μg/g level.

scholarly journals Simultaneous Determination of 17 Sulfonamides and the Potentiators Ormetoprim and Trimethoprim in Salmon Muscle by Liquid Chromatography with Tandem Mass Spectrometry Detection

2007 ◽  
Vol 90 (1) ◽  
pp. 343-348 ◽  
Author(s):  
Ross A Potter ◽  
B Garth Burns ◽  
Jeffrey M van de Riet ◽  
David H North ◽  
Rozina Darvesh
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Fish Tissue ◽  
Reversed Phase ◽  
Tandem Mass ◽  
Relative Standard

Abstract A simple, robust method using liquid chromatography/tandem mass spectrometry (LC/MS/MS) for the simultaneous determination of 17 sulfonamides sulfanilamide (SNL), sulfacetamide (SAA), sulfaguanidine (SGD), sulfapyridine (SPY), sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethoxazole (SOZ), sulfamoxole (SXL), sulfisoxazole (SXZ), sulfamethizole (SML), sulfamethazine (SMZ), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfachloropyridazine (SCP), sulfaquinoxaline (SQX), and sulfadimethoxine (SDM) and 2 potentiators ormetoprim (OMP) and trimethoprim (TMP) in fish tissue has been developed. The analytes were extracted from homogenized fish tissue with wateracetonitrile (50 + 50). The extract was clarified by centrifugation and a portion defatted with hexane. The analytes were partitioned into chloroform and evaporated to dryness. The redissolved residue was applied to a C18 reversed-phase column with a wateracetonitrile (0.1% acetic acid) gradient. All of the compounds were completely separated and detected in <10 min at 30°C using LC/MS/MS. Standard curves were linear over the range of 0.02 to 5 ng injected. The limit of detection varied from 0.1 ng/g for SMZ and OMP to 0.9 ng/g for SXL and SOZ. Recoveries varied from 100% for SDM, SOZ, and SQX and 85% for SMR, OMP, and TMP to approximately 30% for SAA. Relative standard deviations for repeat analysis varied from 4% for SMZ and SCP to 23% for SAA.

Coupling of capillary-channeled polymer (C-CP) fibers for reversed phase liquid chromatography and ESI-MS for the determination of proteins in a urine matrix

2016 ◽  
Vol 8 (48) ◽  
pp. 8410-8419 ◽  
Author(s):  
Lei Wang ◽  
Marissa A. Pierson ◽  
R. Kenneth Marcus
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Reversed Phase ◽  
Ionization Mass ◽  
Reversed Phase Liquid Chromatography ◽  
Esi Ms ◽  
Detection Mode ◽  
Phase Liquid ◽  
Urine Matrix

Electrospray ionization mass spectrometry (ESI-MS) analysis provides a great deal of analytical information as a detection mode when coupled with liquid chromatography (LC) and capillary electrophoresis (CE) separations of proteins.

scholarly journals Determination of Phenolic Compounds in Dietary Supplements and Tea Blends Containing Echinacea by Liquid Chromatography with Coulometric Electrochemical Detection

2003 ◽  
Vol 86 (2) ◽  
pp. 202-208 ◽  
Author(s):  
Wenhong Luo ◽  
Catherina Y W Ang ◽  
Theresa A Gehring ◽  
Thomas M Heinze ◽  
Lawrence J Lin ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Phenolic Compounds ◽  
Dietary Supplements ◽  
Reversed Phase ◽  
Ionization Mass ◽  
Cichoric Acid ◽  
Extraction Solvent ◽  
Caftaric Acid ◽  
Sensitivity And Selectivity

Abstract Analytical methodologies with ultrasonic extraction and liquid chromatography (LC) were developed for the determination of phenolic compounds in dietary supplements containing Echinacea. The phenolic compounds determined by these methods included caftaric acid, chlorogenic acid, cynarin, echinacoside, and cichoric acid. Samples from tablets, capsules, and bags of tea blends were extracted by sonication for ≤30 min with methanol–water (60 + 40). The extracts were centrifuged and filtered, and the filtrates were diluted and analyzed by LC using a reversed-phase column and coulometric electrochemical (EC) detection. The mobile phase was acetonitrile–ammonium formate buffer, pH 3.5 (15.3 + 84.7) containing tetrabutyl ammonium hydrogen sulfate as an ion-pairing reagent. Extraction conditions (e.g., composition of the extraction solvent and sonication time) were optimized for different types of samples. Intra- and interday analytical variations were determined, and intraday analyses were performed by 2 independent analysts using 2 different LC systems. Results were generally comparable. The LC method with EC detection showed better sensitivity and selectivity when compared with LC with ultraviolet detection, although results were similar for the 2 methods for major compounds, i.e., caftaric acid, echinacoside, and cichoric acid. The identities of these major compounds found in samples were confirmed by LC/electrospray ionization mass spectrometry.

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