Plasma phospholipids implicated in the matrix effect observed in liquid chromatography/tandem mass spectrometry bioanalysis: evaluation of the use of colloidal silica in combination with divalent or trivalent cations for the selective removal of phospholipids from plasma

2008 ◽  
Vol 22 (18) ◽  
pp. 2873-2881 ◽  
Author(s):  
Steven T. Wu ◽  
Dale Schoener ◽  
Mohammed Jemal
2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Chaonan Han ◽  
Xiuqin Li ◽  
Hui Jiao ◽  
Yan Gao ◽  
Qinghe Zhang

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the most commonly used method for sulfonamide determination. Its accuracy, however, can be affected by many factors. In this study, sulfadiazine (SDZ), sulfadimidine (SMZ), and sulfadimethoxine (SDM) in milk were selected to investigate an accurate determination method and the potential influencing factors in the use of ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Milk samples were extracted by 25 mL perchloric acid solution (pH = 2) and cleaned up using HLB solid-phase extraction (SPE) cartridges. Four kinds of filters, including PTFE, GHP, nylon, and glass fiber, were compared, and PTFE was selected since it had the best recoveries of target sulfonamides (SAs). Three quantitative methods, including external standard (ES), matrix matching (MM), and isotope dilution mass spectrometry (IDMS), were compared, among which IDMS exhibited the best accuracy. The matrix effect under different mobile phase compositions and of different sample matrices were evaluated and discussed. Ion suppression effects were observed during the determination of all SAs, which got stronger with the increase of the methanol composition percent in the mobile phase. After correction by IDMS, the matrix effect could be neglected. Matrix spiked recoveries at three spiked levels (1 μg/kg, 10 μg/kg, and 20 μg/kg) ranged from 96.8% to 103.8% by IDMS. The expanded relative uncertainties were in the range of 2.02% to 5.75%. The method exhibited wide application range, high accuracy, good stability, and high sensitivity.


Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4598
Author(s):  
Sofie Rutjens ◽  
Siska Croubels ◽  
Siegrid De Baere ◽  
Mathias Devreese

Cefquinome and ceftiofur are β-lactam antibiotics used for the treatment of bacterial infections in swine. Although these antimicrobials are administered intramuscularly, the exposure of the gut microbiota to these cephalosporins is not well described. This exposure can contribute to the emergence and spread of antimicrobials in the environment and to the possible spread of antimicrobial resistance genes. To assess the impact of drug administration on the intestinal excretion of these antimicrobials it is essential to measure the amounts of native compound and metabolites in feces. Two (ultra)-high-performance liquid chromatography-tandem mass spectrometry ((U)HPLC–MS/MS) methods were developed and validated, one for the determination of cefquinome and ceftiofur and the other for the determination of ceftiofur residues, measured as desfuroylceftiofuracetamide, in porcine feces. The matrix-based calibration curve was linear from 5 ng g−1 to 1000 ng g−1 for cefquinome (correlation coefficient (r) = 0.9990 ± 0.0007; goodness of fit (gof) = 3.70 ± 1.43) and ceftiofur (r = 0.9979 ± 0.0009; gof = 5.51 ± 1.14) and quadratic from 30 ng g−1 to 2000 ng g−1 for desfuroylceftiofuracetamide (r = 0.9960 ± 0.0020; gof = 7.31 ± 1.76). The within-day and between-day precision and accuracy fell within the specified ranges. Since β-lactam antibiotics are known to be unstable in feces, additional experiments were conducted to adjust the sampling protocol in order to minimize the impact of the matrix constituents on the stability of the analytes. Immediately after sampling, 500 µL of an 8 µg mL−1 tazobactam solution in water was added to 0.5 g feces, to reduce the degradation in matrix.


2016 ◽  
Vol 8 (38) ◽  
pp. 6903-6908
Author(s):  
Yanyan Hu ◽  
Lu Shen ◽  
Liupeng Wang ◽  
Tingting Yuan ◽  
Yi Sun ◽  
...  

Assessment of the matrix effect by a post-column infusion method and sufficient matrix–analyte separation with a Synergi 4 μm Hydro-RP.


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