کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1200609 1493676 2012 8 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
The evaluation of the applicability of a high pH mobile phase in ultrahigh performance liquid chromatography tandem mass spectrometry analysis of benzodiazepines and benzodiazepine-like hypnotics in urine and blood
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
The evaluation of the applicability of a high pH mobile phase in ultrahigh performance liquid chromatography tandem mass spectrometry analysis of benzodiazepines and benzodiazepine-like hypnotics in urine and blood
چکیده انگلیسی

A sensitive liquid chromatography tandem mass spectrometry method was developed and validated for simultaneous detection of benzodiazepines, benzodiazepine-like hypnotics and some metabolites (7-aminoflunitrazepam, alprazolam, bromazepam, brotizolam, chlordiazepoxide, chlornordiazepam, clobazam, clonazepam, clotiazepam, cloxazolam, diazepam, ethylloflazepate, flunitrazepam, flurazepam, loprazolam, lorazepam, lormetazepam, midazolam, N-desmethylflunitrazepam, nitrazepam, N-methylclonazepam (internal standard), nordiazepam, oxazepam, prazepam, temazepam, tetrazepam, triazolam, zaleplon, zolpidem, zopiclone) in urine and whole blood. Sample preparation was performed on a mixed-mode cation exchange solid phase extraction cartridge. Electrospray ionization was found to be more efficient than atmospheric pressure chemical ionization. The use of a mobile phase of high pH resulted in higher retention and higher electrospray ionization signals than the conventional low pH mobile phases. Considering the benefits of a high pH mobile phase on both chromatography and mass spectrometry, its use should be encouraged. In the final method, gradient elution with 10 mM ammonium bicarbonate (pH 9) and methanol was performed on a small particle column (Acquity C18, 1.7 μm, 2.1 mm × 50 mm). The optimized method was fully validated.


► Several parameters for UFLC–MS/MS analysis of benzodiazepine(-like) hypnotics were studied.
► ESI was more efficient than APCI.
► ESI signal was higher when using high pH mobile phase compared to low pH.
► More retention with a high pH mobile phase than at low pH using RP-LC.
► Considering the benefits of a high pH mobile phase on both LC and MS, its use should be encouraged.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography A - Volume 1249, 3 August 2012, Pages 147–154
نویسندگان
, , ,