کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
6555305 | 1422465 | 2018 | 8 صفحه PDF | دانلود رایگان |
عنوان انگلیسی مقاله ISI
High-throughput determination of valproate in human samples by modified QuEChERS extraction and GC-MS/MS
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موضوعات مرتبط
مهندسی و علوم پایه
شیمی
شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
چکیده انگلیسی
A new high-throughput method was developed for analysis of valproate in human plasma samples by QuEChERS extraction and gas chromatography-tandem mass spectrometry (GC-MS/MS). Plasma samples (0.2â¯ml) spiked with valproate and secobarbital-d5 (internal standard) were diluted with 1.3â¯ml of distilled water. Acetonitrile (1â¯ml) was added followed by 0.4â¯g MgSO4 and 0.1â¯g NaOAC. After a centrifugation step (2000â¯g for 10â¯min), 1â¯ml of the supernatant was transferred to a dispersive-solid phase extraction (dSPE) tube containing 150â¯mg MgSO4 and 50â¯mg C18. This mixture was vortexed and centrifuged at 3000â¯g for 5â¯min, and then the upper layer was evaporated to dryness under a stream of nitrogen. The residue was dissolved in 40â¯Î¼l ethyl acetate, and a 1-μl aliquot was injected into the GC-MS/MS. The GC separation of the compounds was achieved on a fused-silica capillary column Rxi-5Sil MS (30â¯mâ¯Ãâ¯0.25â¯mm i.d.; 0.25-µm film thickness) and detected by MS/MS operating in electron ionization ion source mode. The regression equations showed excellent linearity (râ¯>â¯0.9997) from 50 to 5000â¯ng/ml for plasma, with limit of detection of 10â¯ng/ml. The extraction efficiency of valproate for plasma ranged between 71.2%-103.5%. The coefficient of variation was <18.5%. The method was successfully applied to actual analyses of an autopsy case. This method can be useful for simple and reliable measurements of valproate in clinical and toxicological analyses; it can be integrated in screening and simultaneous determination methods for multiple drugs and poisons in the further studies.
ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Legal Medicine - Volume 31, March 2018, Pages 66-73
Journal: Legal Medicine - Volume 31, March 2018, Pages 66-73
نویسندگان
Shun Mizuno, Xiao-Pen Lee, Masaya Fujishiro, Takaaki Matsuyama, Miho Yamada, Yuki Sakamoto, Maiko Kusano, Kei Zaitsu, Chika Hasegawa, Iwao Hasegawa, Takeshi Kumazawa, Akira Ishii, Keizo Sato,