RESUMEN
This paper describes an assay for the determination of glyphosate (GLYP), glyphosate metabolites [(aminomethyl) phosphonic acid] (AMPA), and glufosinate (GLUF) in human serum. After protein precipitation using acetonitrile and solid-phase extraction, serum samples were derivatized and analyzed by gas chromatography-mass spectrometry (GC-MS). The assay was linear over a concentration range of 3-100.0 microg/ml for GLYP, AMPA, and GLUF. The overall recoveries for the three compounds were >73%. The intra- and inter-day variations were <15%. Precision and accuracy were 6.4-10.6% and 88.2-103.7%, respectively. The validated method was applied to quantify the GLYP and AMPA content in the serum of a GLYP-poisoned patient. In conclusion, the method was successfully applied for the determination of GLYP and its metabolite AMPA in serum obtained from patient of GLYP-poisoning.
Asunto(s)
Aminobutiratos/sangre , Cromatografía de Gases y Espectrometría de Masas/métodos , Glicina/análogos & derivados , Herbicidas/sangre , Organofosfonatos/sangre , Aminobutiratos/envenenamiento , Aminobutiratos/orina , Estabilidad de Medicamentos , Glicina/sangre , Glicina/envenenamiento , Glicina/orina , Herbicidas/envenenamiento , Herbicidas/orina , Humanos , Isoxazoles , Modelos Lineales , Masculino , Persona de Mediana Edad , Organofosfonatos/orina , Estándares de Referencia , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Intento de Suicidio , Tetrazoles , GlifosatoRESUMEN
A rapid headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method has been developed for the determination of metaldehyde in human serum samples. Metaldehyde is extensively used as a molluscicide for the control of slugs and snails, and cases of metaldehyde poisoning have been reported. Metaldehyde was headspace-extracted on a polydimethylsiloxane (PDMS) fiber at 70 degrees C for 25 min, desorbed, and analyzed rapidly by GC-MS. The method was validated for limit of detection (LOD), linearity, precision, and recovery. Although the recovery of the sample was very low, the method itself was rapid with a low detection limit of 0.25 microg/ml, R.S.D. value 12.6%, and linearity range 0.5-25.0 microg/ml (r(2)=0.999). The results demonstrated that the SPME-GC-MS method for the analysis of metaldehyde is simple, rapid, solvent-free, and does not require any pre-analysis conversions.
Asunto(s)
Acetaldehído/análogos & derivados , Cromatografía de Gases y Espectrometría de Masas/métodos , Microextracción en Fase Sólida/métodos , Acetaldehído/sangre , Acetaldehído/envenenamiento , Dimetilpolisiloxanos , Estabilidad de Medicamentos , Femenino , Humanos , Modelos Lineales , Moluscocidas/sangre , Moluscocidas/envenenamiento , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Intento de Suicidio , Adulto JovenRESUMEN
We performed D2 low anterior resection in a patient with stage I rectal cancer [pathological diagnosis: proper muscle (pm) invasion, n0, lymphatic invasion (ly), (-); venous invasion (v), (-); anal margin, (-)]. The tumor recurred at the anastomotic site approximately one year later and was treated with Miles' operation [pm, n0, ly (+); v (-); deep border of the primary tumor (-)]. The tumor marker CEA increased to 50.4 ng/ml at four months after surgery and pelvic local recurrence was detected. Since then, the patient has been receiving chemoradiotherapy on an out-patient basis. Cytokeratin immunostaining of all the lymph nodes collected during the two operations showed clusters of occult neoplastic cells (ONCs) in the perinodal fat around the nodes harvested at the first operation. These findings suggest that the risk of local recurrence of rectal cancer is increased even in stage I disease if ONCs are found in the perinodal fat. Further studies are required to examine the relationship between local recurrence and extranodal ONCs in patients with primary rectal cancer.