NDLI: Separation of 9 Sulfonamide Drugs in ≈4 Min by Ultra-High Performance Supercritical Fluid Chromatography (UHPSFC): with a Feasibility Study for Detection in Milk

Content Provider	Springer Nature Link
Author	Berger, Terry A. Berger, Blair K.
Copyright Year	2013
Abstract	Nine widely used veterinary sulfonamide drugs were baseline separated (R s ≥1.5) in just over 4 min using a 3 × 100 mm, 1.8 μm RX-Sil column, with 9.2 % methanol in carbon dioxide, at 110 bar and 30 °C, with direct UV detection at 260 nm using a 3 mm, 2 μL tapered flow cell. Pressure drop was only 172 bar. Optimization was difficult due to the similarity in structures. Small changes in modifier concentration, temperature and pressure, each tended to improve the resolution of some peak pairs but degraded the resolution of others. There were four critical pairs, each responding differently to changes in conditions. Optimization was performed by plotting resolution between pairs as a function of modifier concentration first, temperature second, and outlet pressure third. Retention time was then minimized by changing flow rate. The estimated limit of quantitation (LOQ, S/N >10), for direct injections, was ≈200–400 ng/g of each, inadequate for regulatory requirements. Solid phase extraction (SPE) attempted to pre-concentrate samples spiked with sulfamethazine by ≈20:1. From water, the limit of detection (LOD) was ≈2.7 ng/mL with LOQ ≈9 ng/mL using UV at 260 nm. The LOD for milk was 6.2 ng/mL, and LOQ was 20.1 ng/mL. A better pre-concentration step or a more sensitive detector such as MS–MS is required. Even with these inadequacies, SFC was shown to be a feasible, faster, “greener” alternative to HPLC for the separation of these drugs.
Starting Page	1631
Ending Page	1639
Page Count	9
File Format	PDF
ISSN	00095893
Journal	Chromatographia
Volume Number	76
Issue Number	23-24
e-ISSN	16121112
Language	English
Publisher	Springer Berlin Heidelberg
Publisher Date	2013-08-29
Publisher Place	Berlin, Heidelberg
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Ultra-high performance supercritical fluid chromatography (UHPSFC) Sulfonamide antimicrobials Method development Resolution Critical pairs Isocratic Milk UV detection Chromatography Proteomics Pharmacy Laboratory Medicine
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Analytical Chemistry Biochemistry Clinical Biochemistry

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