scholarly journals Development of a Fast Liquid Chromatography Coupled to Mass Spectrometry Method (LC-MS/MS) to Determine Fourteen Lipophilic Shellfish Toxins Based on Fused–Core Technology: In-House Validation

Marine Drugs ◽  
2021 ◽  
Vol 19 (11) ◽  
pp. 603
Author(s):  
Araceli E. Rossignoli ◽  
Carmen Mariño ◽  
Helena Martín ◽  
Juan Blanco
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Phytoplankton Species ◽  
Core Technology ◽  
Highly Sensitive ◽  
Repeatability And Reproducibility ◽  
Lipophilic Toxins ◽  
Fast Liquid Chromatography

Prevalence and incidence of the marine toxins (paralytic, amnesic, and lipophilic toxins) including the so-called emerging toxins (these are, gymnodimines, pinnatoxins, or spirolides among others) have increased in recent years all over the world. Climate change, which is affecting the distribution of their producing phytoplankton species, is probably one of the main causes. Early detection of the toxins present in a particular area, and linking the toxins to their causative phytoplankton species are key tools to minimize the risk they pose for human consumers. The development of both types of studies requires fast and highly sensitive analytical methods. In the present work, we have developed a highly sensitive liquid chromatography-mass spectrometry methodology (LC-MS/MS), using a column with fused-core particle technology, for the determination of fourteen lipophilic toxins in a single run of 3.6 min. The performance of the method was evaluated for specificity, linearity, precision (repeatability and reproducibility) and accuracy by analysing spiked and naturally contaminated samples. The in-house validation was successful, and the limit of detection (LOD) and quantification (LOQ) for all the toxins were far below their regulatory action limits. The method is suitable to be considered in monitoring systems of bivalves for food control.

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.

Liquid chromatography-mass spectrometry determination of iloperidone on rat dried blood spots: application to pharmacokinetics

2017 ◽  
Vol 9 (39) ◽  
pp. 5749-5756
Author(s):  
R. Nageswara Rao ◽  
K. Guru Prasad ◽  
Sara Khalid ◽  
K. S. Praneetha ◽  
Dilip Dodda ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Dried Blood Spots ◽  
Liquid Chromatography Mass Spectrometry ◽  
Spectrometry Method ◽  
Mass Spectrometry Method ◽  
Blood Spots ◽  
Chromatography Mass Spectrometry ◽  
Highly Sensitive

A simple, rapid and highly sensitive liquid chromatography-mass spectrometry method was developed and validated for analysis of iloperidone on rat dried blood spots.

scholarly journals Quantitative LC/MS-MS Determination of Sulfonamides and Some Other Antibiotics in Honey

2002 ◽  
Vol 85 (4) ◽  
pp. 853-860 ◽  
Author(s):  
Anton Kaufmann ◽  
Sven Roth ◽  
Bianca Ryser ◽  
Mirjam Widmer ◽  
Dominik Guggisberg
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Rapid Method ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Abstract A simple and rapid method was developed for the determination of 20 antibiotics (sulfonamides, tetracyclines, and flumequine) in honey by liquid chromatography tandem mass spectrometry. The proposed method is sensitive (limit of detection 0.5 to 10 ppb for the various antibiotics) and selective. A hydrolysis step ensures the liberation of sugar-bound sulfonamides. The approach has been used to analyze some 300 honey samples. A number of them were found to have exceeded the Swiss limit of 50 ppb.

scholarly journals Simultaneous Determination of Nine Bioactive Constituents of Caulis Lonicerae Japonicae by High-Performance Liquid Chromatography Coupled with Mass Spectrometry

2008 ◽  
Vol 3 (5) ◽  
pp. 1934578X0800300 ◽  
Author(s):  
Hui-Jun Li ◽  
Zheng-Ming Qian ◽  
Ping Li ◽  
Mei-Ting Ren ◽  
Jun Chen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Quinic Acid ◽  
Column Temperature ◽  
Caffeoyl Quinic Acid

A new high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) method has been developed for the simultaneous determination of nine major compounds, namely chlorogenic acid (1), caffeic acid (2), sweroside (3), loganin (4), secoxyloganin (5), 3,5-di- O-caffeoyl quinic acid (6), luteolin-7- O-glucoside (7), rutin (8) and 3,4-di- O-caffeoyl quinic acid (9), in Caulis Lonicerae Japonicae (CLJ), a commonly used traditional Chinese medicinal herb. The separation was achieved on a C-18 column (250 × 4.6 mm, 5.0 μm) with a column temperature of 30°C and a flow-rate of 0.8 mL/min. The mobile phase was composed of (A) aqueous formic acid (0.1%, v/v) and (B) methanol, using a gradient elution of 30% B for 0-13 min, 30–40% B for 13–17 min, and 40–49% B for 17–30 min. The limit of detection ( S/ N = 3) ranged from 0.8 to 5.1 ng/mL and the limit of quantification ( S/ N = 10) varied from 3.4 to 16.9 ng/mL. All calibration curves showed good linear regression ( r2 > 0.9976) within the test ranges. The intra- and inter-day precisions, as determined from sample solutions, were below 2.2 and 4.3%, respectively. The recoveries for nine compounds were within 91.3 and 104.2%. This proposed method has been successfully applied to evaluation of commercial samples of CLJ from different markets in China, which provides a new basis of assessment of the quality of the herbal drug.

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