کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
7614900 | 1493979 | 2018 | 32 صفحه PDF | دانلود رایگان |
عنوان انگلیسی مقاله ISI
Splitless hyphenation of SFC with MS by APCI, APPI, and ESI exemplified by steroids as model compounds
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کلمات کلیدی
APCISGFSGTMRMUHPLCRMSDGTAPPIACNTBCDGFSFCNH4OACLOQPrOHESIS/N - S / NAmmonium acetate - استات آمونیومEndogenous steroids - استروئیدهای اندوژنAcetonitrile - استونیتریلFormic acid - اسید فرمیکGas phase acidity - اسیدیته فاز گازIonization energy - انرژی یونیزاسیونToluene - تولوئنCorona current - جریان کروناLOD یا Limit of detection - حد تشخیصAmmonium formate - فرمیت آمونیومMethanol - متانولlimit of quantification - محدودیت اندازه گیریlimit of detection - محدودیت تشخیصMeOH - مونroot mean square - میانگین مربع ریشهsignal to noise ratio - نسبت سیگنال به نویزmultiple reaction monitoring - نظارت چندگانه چندگانهproton affinity - وابستگی پروتونPropan-2-ol - پروپان 2-الhigh performance liquid chromatography - کروماتوگرافی مایع با کارایی بالاHPLC - کروماتوگرافی مایعی کاراGas chromatography - کروماتوگرافی گازی
موضوعات مرتبط
مهندسی و علوم پایه
شیمی
شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
چکیده انگلیسی
A systematic evaluation of splitless hyphenation of supercritical fluid chromatography (SFC) with mass spectrometry (MS) was performed using different techniques for ambient pressure ionization. Interfaces commonly known from HPLC-MS/MS, i.e. electrospray ionization (ESI), atmospheric pressure chemical ionization (APCI), and atmospheric pressure photo ionization (APPI), were tested for their suitability in SFC-MS/MS. A triple quadrupole MS was used for data evaluation in a targeted multi-analyte design using endogenous steroids as model compounds. Individual optimization of the ionization parameters was performed in multi-dimensional design for best support of ionization in all three techniques. A post-column make-up was used to avoid analyte precipitation in the transfer capillary but also to support ionization independently from mobile phase composition. Buffer choice and concentration as well as temperature were found crucial in ESI and APCI. Best results for the multi-analyte method were obtained in both techniques using ammonium fluoride as make-up buffer. Instead of buffer solutions different organic solvents were used as dopants in APPI to support ionization. The mobile phase constituent isopropanol was already found to support ionization in APPI, however, for many analytes the addition of toluene resulted in superior results in terms of intensity. Comparing the optimized methods in terms of limit of detection (LOD), limit of quantification (LOQ), and sensitivity (slope of calibration curve) ESI was the best choice for the multiple analyte design. Only a few analytes resulted in a different optimum ionization, if focused on separately. In terms of linear dynamic range, APCI and APPI proved superior to ESI, where calibration over the whole range of concentrations (from LOD up to 5000â¯pgâ¯ââ¯Î¼Lâ1) required quadratic regression.
ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography B - Volume 1091, 1 August 2018, Pages 67-78
Journal: Journal of Chromatography B - Volume 1091, 1 August 2018, Pages 67-78
نویسندگان
Maria Kristina Parr, Bernhard Wüst, Juliane Teubel, Jan Felix Joseph,