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Determination of glyphosate and glufosinate in human serum by monospin TiO extraction and liquid chromatography–tandem mass spectrometry

Saito Takeshi, Namera Akira, Tsuji Tomoatsu, Noguchi Wataru, Inokuchi Sadaki

Acta Chromatographica

2020

Vol. 32, no. 1

10--15

We developed and validated an assay for determination of glyphosate (GLYP) and glufosinate (GLUF) in human serum. Serum samples were extracted by using a MonoSpin® TiO column and analyzed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). MonoSpin® TiO tends to specifically bind to phosphate groups. The assay was linear over a concentration range of 1–250 μg/mL. The recoveries for the 2 compounds were 1.6%–2.3%. The intra- and inter-day variations were <15%. Precision and accuracy were 5.6%–12.7% and 97.0%–103.9%, respectively. The validated method was applied to quantify the GLYP and GLUF content in the serum of GLYP and GLUF-poisoned patients. In conclusion, the method was successfully applied for accurate determination of GLYP and GLUF in serum obtained from patients with GLYP and GLUF poisoning.

Eruption age of Kannabe volcano using multi-dating: Implications for age determination of young basaltic lava flow

Shitaoka Yorinao, Saito Takeshi, Yamamoto Junji, Miyoshi Masaya, Ishibashi Hidemi, Soda Tsutomu

Geochronometria

2019

Vol. 46, no. 1

49--56

We estimated the eruption age of Kannabe volcano, located in southwestern Japan. Although the eruption age had been estimated using tephrochronology and K-Ar dating, the precision of its age determination left some room for improvement. The latest eruption age of Kannabe volcano is well constrained by wide spread tephras to ca. 7.2–30 ka. We applied paleomagnetic dating to a basaltic lava and optically stimulated luminescence (OSL) dating to a soil layer, which are associated with the Kannabe volcano. The soil layer above the Kannabe scoria was newly dated to be 21 ± 6 ka, as inferred from OSL dating. We also made paleomagnetic investigation to estimate the eruption age of the Kannabe basaltic lava. Paleomagnetic data of 23 rock samples from six locations in the Kannabe basaltic lava showed good mutual agreement. The average of remanent magnetizations yields declination of 0.3° and inclination of 65.9° with 95% confidence limit of 2.7°. This paleomagnetic direction with a relatively steep inclination is thought to be correlated with the paleomagnetic secular variation data of sediments in Lake Biwa at ca. 21.5 ka. Based on that information from multi-dating, we inferred that the Kannabe volcano erupted at ca. 22 ka. This result presents profound scientific implications for the precise age determination of young basaltic lava flow, for which few dating methods exist.

High-throughput monospin extraction for quantification of cardiovascular drugs in serum coupled to high-performance liquid chromatography–mass spectrometry

Namera Akira, Saito Takeshi, Seki Yoshimoto, Mizutani Taro, Murata Kazuhiro, Nagao Masataka

Acta Chromatographica

2019

Vol. 31, no. 4

294--298

A novel method coupling spin column extraction with high-performance liquid chromatography–mass spectrometry was developed for simultaneous extraction of β-blockers and calcium channel blockers from human serum. Sample loading, washing, and elution were accomplished via centrifugation of the column, in which mixed-mode monolithic silica bonded to a C18 reversed phase, and a cation-exchange phase was packed in a spin column. The serum sample (0.2 mL) pH was adjusted to 3 and the analytes adsorbed onto the column were eluted with 0.1 mL MeOH containing 2% NH3. The recoveries of the tested drugs were 76–108%. A linear curve was observed up to a concentration of 500 ng/mL of the target drugs in serum (r2 > 0.996). The intra-day relative standard deviations at three different concentrations were 0.6–9.6%. The limits of detection were 2 ng/mL. The proposed method was successfully applied to clinical and forensic cases.