کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
7626668 | 1494582 | 2018 | 10 صفحه PDF | دانلود رایگان |
عنوان انگلیسی مقاله ISI
Comparative evaluation of ICP sample introduction systems to be used in the metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS
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کلمات کلیدی
ESIKEDU.S. FDALOQGMPU.S. Food and Drug Administration - اداره غذا و داروی ایالات متحدهCapillary electrophoresis - الکتروفورزمویرگیKinetic energy discrimination - تبعیض انرژی جنبشیUltraviolet detection - تشخیص ultra violetGood Manufacturing Practice - تمرین تولید خوبLOD یا Limit of detection - حد تشخیصInternal Diameter - قطر داخلیlimit of quantification - محدودیت اندازه گیریlimit of detection - محدودیت تشخیصMetabolite profiling - پروفیل متابولیتGas chromatography - کروماتوگرافی گازیhigh resolution - کیفیت بالاSpeciation - گونه زاییelectrospray ionization - یونیزاسیون الکترو اسپری
موضوعات مرتبط
مهندسی و علوم پایه
شیمی
شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
چکیده انگلیسی
A systematic evaluation of four different ICP sample introduction systems to be used in the context of metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS was carried out using diclofenac and its major metabolite, 4â²-hydroxy-diclofenac, as model compounds. The strict requirements for GMP validation of chromatographic methods in the pharmaceutical industry were adhered to in this context. The final aim of this investigation is an extension of the applicability and validatability of HPLC-ICP-MS in the field of pharmaceutical R&D. Five different gradient programmes were tested while the baseline peak width (wb), peak capacity (P), USP tailing factor (As) and USP signal-to-noise ratio (USP S/N) were determined as major indicators of the chromatographic performance and the values obtained were compared to the corresponding FDA recommendations (if applicable). Four different ICP-MS sample introductions systems were investigated involving two units typically working at higher flow rates (â¼1.0â¯mLâ¯minâ1) and another two systems working at lower flow rates (â¼0.1â¯mLâ¯minâ1). Optimal conditions with potential for applicability under GMP conditions were found at a mobile phase flow rate of 1.0â¯mLâ¯minâ1 by using a pneumatic micro-flow LC nebulizer mounted onto a Peltier-cooled cyclonic spray chamber cooled to â1â¯Â°C for sample introduction. Under these conditions, HPLC-ICP-MS provided a chromatographic performance similar to that of HPLC with UV detection. The peak shape (USP tailing factorâ¯=â¯1.1-1.4) was significantly improved compared to that obtained with the Peltier-cooled Scott-type spray chamber. Two alternative sample introduction systems â a POINT® and a High-Temperature Torch-Integrated Sample Introduction System (hTISIS) â were also tested at a flow rate of 0.1â¯mLâ¯minâ1 using a chromatographic column with 1.0â¯mm ID. Although these systems allowed the peak shape to be improved compared to that obtained with the traditional Scott-type spray chamber, the limits of detection and of quantification achievable were strongly compromised due to the significantly lower sensitivity observed for Cl. In addition to a comparison of the aforementioned sample introduction systems, also the effect of spray chamber temperature was evaluated and it was demonstrated that proper temperature control plays an essential role in the optimization of HPLC-ICP-MS methods.
ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Pharmaceutical and Biomedical Analysis - Volume 153, 10 May 2018, Pages 135-144
Journal: Journal of Pharmaceutical and Biomedical Analysis - Volume 153, 10 May 2018, Pages 135-144
نویسندگان
Balázs Klencsár, Carlos Sánchez, Lieve Balcaen, José TodolÃ, Frederic Lynen, Frank Vanhaecke,