High‐throughput 96‐well solid‐phase extraction for preparation of tetracycline followed by liquid chromatography and mass spectrometry analysis

Author(s):  
Kang Chen ◽  
Jie Wang ◽  
Shiyan Li ◽  
Yang Wang ◽  
Yiqi Zhang ◽  
...  
2020 ◽  
Vol 25 (1) ◽  
Author(s):  
Hiroshi Nomura ◽  
Risa Hamada ◽  
Isao Saito ◽  
Kunihiko Nakane ◽  
Ritsuko Sawa ◽  
...  

Abstract Background Glyphosate and its salt formulations are nonselective herbicides that have been extensively used worldwide, both for residential and agricultural purposes. The possible carcinogenicity and teratogenicity of glyphosate remain to be elucidated. We developed a sensitive and high-throughput analytical method for urinary glyphosate using liquid chromatography-tandem mass spectrometry with the aim of contributing to glyphosate exposure assessment in epidemiological studies. Methods After urine dilution (creatinine matching dilution to 0.05 g creatinine/L), glyphosate was extracted using two types of solid phase extraction columns (SCX and NH2) with automated sample preparation instruments. The eluate was dried and dissolved in the mobile phase, followed by liquid chromatography-tandem mass spectrometry analysis. The optimized method was applied to urine samples obtained from 54 Japanese adults and children. Results The results from the validation study demonstrated good recoveries (91.0-99.6%), within- and between-run precisions (< 15%), low detection limits (0.1 μg/L), and lower limit of quantification (0.3 μg/L). The detection frequency and median concentration of the urinary glyphosate in Japanese subjects were 59% and 0.25 μg/L (0.34 μg/g creatinine). Conclusions Our reliable determination method was successful in measuring urinary glyphosate concentration. Moreover, this is the first biomonitoring report of urinary glyphosate levels in the Japanese general population.


2003 ◽  
Vol 86 (5) ◽  
pp. 941-946 ◽  
Author(s):  
Giorgio Famiglini ◽  
Helga Trufelli ◽  
Elisabetta Pierini ◽  
Elisa De Simoni ◽  
Filippo Mangani ◽  
...  

Abstract Our recent on-line solid-phase extraction (SPE) device for micro-liquid chromatography, known as micro-solid-phase extraction (μSPE), was compared with traditional SPE for the analysis, from aqueous samples, of 4 pesticides belonging to different classes. Two different kinds of adsorbents, C18 and graphitized carbon black, were tested. A 2-stage ion trap mass spectrometer, equipped with homemade microflow electrospray ion (ESI) source, was used. Detection limits with a signal-to-noise ratio of 3:1 for both extraction methods were in the range of 0.1 μg/L for all compounds. However, better recoveries were obtained when μSPE traps were used.


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