scholarly journals Assessing the matrix effects of pigmented and non-pigmented salmon during multi-residue antibiotic analysis with liquid chromatography coupled to tandem mass spectrometry

2021 ◽  
Author(s):  
Shiva Emami ◽  
Ameer Y Taha
Keyword(s):  
Liquid Chromatography ◽  
Sockeye Salmon ◽  
Matrix Effects ◽  
Solid Phase ◽  
Quechers Method ◽  
Modified Quechers ◽  
Ms Analysis ◽  
Hydrophilic Lipophilic Balance ◽  
The Matrix ◽  
Matrix Components

Several validated methods exist for the quantitation of antibiotics in seafood with ultra-high pressure liquid chromatography coupled with tandem spectrometry (UPLC-MS/MS). To our knowledge, none have explored the effects of co-eluting matrix components on the accuracy of quantitation. Such matrix effects could disproportionally change the ionization of analytes and their respective surrogate/internal standards during UPLC-MS/MS analysis, resulting in over- or under-estimation of antibiotic values. In this study, we measured matrix effects, alongside extraction recoveries for 30 antibiotics and their respective class-specific surrogate standards in Sockeye, King and Ivory (non-pigmented) salmon extracted using the QUEChERS method. A modified QUEChERS method involving dispersive or hydrophilic-lipophilic balance (HLB) solid phase extraction (SPE) was also tested on Sockeye salmon. Despite acceptable extraction recoveries for most antibiotics extracted using the QUEChERS method, significant matrix effects were observed for most antibiotic standards. Dispersive or HLB SPE clean-up did not improve analyte recoveries from Sockeye salmon, and in some cases, increased matrix effects. Accuracy and sensitivity were reduced when matrix effects were high. Our results demonstrate that matrix components in salmon cause matrix effects on antibiotics during UPLC-MS/MS analysis which could impact the accuracy and sensitivity of the analysis.

scholarly journals Determination of Residual Triflumezopyrim Insecticide in Agricultural Products through a Modified QuEChERS Method

Foods ◽  
2021 ◽  
Vol 10 (9) ◽  
pp. 2090
Author(s):  
Sung-Min Cho ◽  
Han-Sol Lee ◽  
Ji-Su Park ◽  
Su-Jung Lee ◽  
Hye-Sun Shin ◽  
...  
Keyword(s):  
Analytical Method ◽  
Matrix Effects ◽  
Solid Phase ◽  
Reference Method ◽  
Quechers Method ◽  
Modified Quechers ◽  
Relative Standard ◽  
The Matrix ◽  
Food Commodities

A rapid and simple analytical method for triflumezopyrim, a new class of mesoionic insecticides and commercialized molecules from DuPont, was developed with a modified QuEChERS method. The pH adjustment was used to improve the extraction efficiency of acetonitrile solvent, and dispersive solid-phase extraction was employed for the clean-up process. The five selected food commodities were used to verify the present optimized method, which displayed good linearity with an excellent correlation coefficient (R2 = 0.9992–0.9998) in the 0.003–0.30 mg/kg calibration range. The method limits of detection (LOD) and quantification (LOQ) were determined to be a value of 0.003 and 0.01 mg/kg, respectively. The mean recovery for the triflumezopyrim was in the 89.7–104.3% range. The relative standard deviations were ≤9.8% for intra- (n = 5) and inter-day (n = 15) precisions at concentrations of 0.01, 0.1, and 0.5 mg/kg in the five representative samples. The matrix effect has been calculated to confirm the effect during ionization of the analyte in the UPLC-MS/MS. The matrix effects of the instrumental analysis showed that triflumezopyrim was less susceptible to matrices. The proposed analytical method in this study has effectively improved the accuracy, selectivity, and sensitivity for the determination of triflumezopyrim in agricultural commodities; therefore, it can serve as a reference method for the establishment of maximum residue limits (MRLs).

Determination of Cannabinoids in Breast Milk Using QuEChERS and Ultra-Performance Liquid Chromatography and Tandem Mass Spectrometry

2019 ◽  
Vol 43 (9) ◽  
pp. 746-752 ◽  
Author(s):  
Rhea S Ramnarine ◽  
Justin L Poklis ◽  
Carl E Wolf
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Breast Milk ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Quechers Method ◽  
Modified Quechers ◽  
High Lipid ◽  
The Matrix

Abstract Use of marijuana and cannabinoids has been on the rise in recent years, including in childbearing women. This has resulted in cannabinoids being more frequently identified in breast milk as a result of its high lipid content and cannabinoids having a high lipophilicity, thereby exposing the breastfeeding infant to cannabinoids and other marijuana constituents. Presented is a method for the analysis of Δ9-tetrahydrocannabinol (THC), cannabinol (CBN) and cannabidiol (CBD) in breast milk. THC, CBN, CBD and their isotopically labeled standards were extracted from breast milk using a modified QuEChERS method and analyzed using ultra-performance liquid chromatography and tandem mass spectrometry. As a result of the high lipid content of breast milk, saponification of the lipids was necessary to improve overall extraction efficiency. The process efficiency percentage for THC, CBD and CBN are 55%, 80% and 25%, respectively. The recovery percentage for THC, CBD and CBN are 95%, 118% and 85%, respectively. The matrix effect percentage for THC, CBD and CBN are 53%, 66% and 26%, respectively. Linearity was assessed from 1 to 100 ng/mL for THC, CBN and CBD and had r2 > 0.996. Validation controls were prepared at 1, 3, 20, 80 and 300 ng/mL (dilution control), and the bias was determined to be less than ±20% with %CVs <15% for all controls. Due to the limited access of genuine breast milk for routinely preparing matrix matched calibration and control materials, Enfamil® Premium™ Newborn Infant Formula (0–3 months) was evaluated as a breast milk substitute. No significant differences were observed for THC, CBN and CBD using either breast milk or formula as the matrix; thus, it was determined to be an acceptable breast milk matrix substitute. The modified QuEChERS method was determined to be a robust, reliable method for the determination of THC, CBN and CBD in breast milk.

Determination of Major Phytohormones in Fourteen Different Seaweeds Utilizing SPE–LC–MS/MS

2019 ◽  
Vol 58 (2) ◽  
pp. 98-108 ◽  
Author(s):  
Sibel Yalçın ◽  
Emine Şükran Okudan ◽  
Özge Karakaş ◽  
Ayşe Nur Önem
Keyword(s):  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Tandem Mass ◽  
Mass Detection ◽  
Hydrophilic Lipophilic Balance ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

Abstract Analysis of plant growth regulators (PGRs) should be approached by considering their extremely low concentrations and serious interfering effects that result from the matrix of various plant tissues. In the current research, the separation and simultaneous determination of different classes of phytohormones in 14 seaweeds collected from Turkey seashores were achieved by using solid-phase extraction (SPE) followed by a rapid and sensitive liquid chromatography tandem mass detection method. OASIS HLB (Hydrophilic-Lipophilic Balance) cartridges were successfully used for SPE process to eliminate the matrix effect and enhance the PGRs including zeatin, benzyl amino purine, indole-3-acetic acid, abscisic acid and gibberellic acid within partially different polarities. Based on the optimized experimental conditions, the method presented excellent performance related to linearity (r, 0.9996–0.9999) within the ranges of 0.5–500 ng/mL, relative standard deviation values ((1.43–2.01) for intraday and (2.36–3.50) for interday)), the limit of detection (0.01–0.84 μg/L) and the limit of quantification (0.02–2.76 μg/L). The obtained results confirm that the SPE–liquid chromatography/tandem mass spectrometry method performed is highly effective and convenient for routine analyses of trace amounts of the tested phytohormones in seaweeds and any other plant samples as well.

A Modified QuEChERS Extraction and LC-MS/MS Method for the Determination of Pesticide Residues in Curry Leaves (Murraya koenigii)

2019 ◽  
Vol 6 (1) ◽  
pp. 30-41
Author(s):  
Ranjith Arimboor ◽  
Karunkara Ramakrishna Menon ◽  
Natarajan Ramesh Babu ◽  
Haneesh Chandran
Keyword(s):  
Sample Preparation ◽  
Matrix Effect ◽  
Retention Time ◽  
Pesticide Residues ◽  
Mobile Phase ◽  
Preparation Technique ◽  
Modified Quechers ◽  
Curry Leaves ◽  
Ms Analysis ◽  
The Matrix

Background:Increased consumer demand for curry leaves free from pesticides demands fast and reliable analytical methods for the analysis of pesticide residues.Objective:The optimization of a QuEChERS based sample preparation technique with improved analytical accuracy by removing interfering matrix components for LC-MS/MS analysis of pesticide residues from curry leaves.Methods:A modified QuEChERS solid phase extraction method was developed and validated for the analysis of 26 pesticides in fresh and dried curry leaves. The effects of the sample preparation steps and column retention time on the matrix suppression of analyte ions were also evaluated.Results:Validation parameters were found within an acceptable range. The matrix effect evaluation studies showed that the QuEChERS sample preparation was able to minimize the ion suppression of analytes due to co-eluting matrix of components and that a d-SPE clean up step had major role in reducing matrix effect. The gradient mobile phase with longer retention time for analytes resulted in comparatively lesser matrix effects than the isocratic mobile phase of non-polar nature. Even after the clean up, a considerable number of compounds had more than 20% reduction in their MS response in the gradient mobile phase.Conclusion:This study emphasized the need of proper sample clean up before a LC-MS/MS analysis and the usage of matrix matched standards and mobile phase that ultimately results in an appropriate analyte separation in reasonable retention times.

scholarly journals Pressurized Solvent Extraction with Ethyl Acetate and Liquid Chromatography—Tandem Mass Spectrometry for the Analysis of Selected Conazole Fungicides in Matcha

Toxics ◽  
2018 ◽  
Vol 6 (4) ◽  
pp. 64 ◽  
Author(s):  
Renata Raina-Fulton ◽  
Aisha Mohamad
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Solvent Extraction ◽  
Matrix Effects ◽  
Tandem Mass ◽  
Esi Ms ◽  
Signal Suppression ◽  
Target Analytes ◽  
Matrix Components ◽  
Pressurized Solvent Extraction

The extraction of powdered nutraceuticals is challenging due to the low water content and high concentration of matrix components that can lead to significant matrix effects in liquid chromatography-positive ion electrospray ionization-tandem mass spectrometry (LC-ESI+-MS/MS). In this study we assess the feasibility of using pressurized solvent extraction with ethyl acetate to reduce the co-extraction of polar matrix components. Pigment attributed to chlorophyll was removed with in-cell clean-up utilizing Anasorb 747, Florisil®, and C18. Visible inspection of the extracts showed that pigment was removed from matcha, a powdered green tea sample. Pressurized solvent extraction with in-cell clean-up can be utilized to remove pigments from powdered samples such as nutraceuticals. Average matrix effect of the 32 target analytes that observed mass spectrometric signal suppression or soft MS signal enhancement was −41 ± 19% with the majority of analytes having a protonated molecular ion with m/z of 250 to 412. As generally moderate signal suppression was observed for conazole fungicides and structurally related compounds analyzed by LC-ESI+-MS/MS, it is recommended that matrix matched or standard addition calibration is used for quantitation. Catachins, other polyphenols, and caffeine are expected to contribute to the matrix effects observed in LC-ESI+-MS/MS. Diniconazole, fenbuconazole, and tebufenozide were the only target analytes with severe MS signal enhancement. Low levels (0.002–0.004 mg/kg) of prothioconazole-desthio and flusilazole were detected, along with trace levels of tebuthiuron in matcha.

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