Expanding current applications and permitting the analysis of larger intact samples by means of a 7 mm CMP–NMR probe. Issue 14 (17th June 2021)

• Record Type: Journal Article
• Authors: Ning, Paris; Lane, Daniel; Ghosh Biswas, Rajshree; Jenne, Amy; Bastawrous, Monica; Soong, Ronald; Schmidig, Daniel; Frei, Thomas; De Castro, Peter; Kovacevic, Ivan; Graf, Stephan; Wegner, Sebastian; Bermel, Wolfgang; Busse, Falko; Kuehn, Till; Kuemmerle, Rainer; Struppe, Jochem; Fey, Michael; Stronks, Henry J.; Monette, Martine; Simpson, Myrna J.; Simpson, André J.
• Is Part Of: Analyst. Volume 146:Issue 14(2021)
• Page Start: 4461
• Page End: 4472
• Publication Date: 2021-06-17
• Subjects: Chemistry, Analytic -- Periodicals; 543
• DOI: 10.1039/d1an00809a
• Languages: English
• ISSNs: 0003-2654

Abstract

Abstract : With a larger sample size, 7 mm CMP–NMR can identify and distinguish components in different phases within a softgel capsule of hydroxyzine hydrochloride. The capsule would not fit in a 4 mm probe. Abstract : Comprehensive multiphase NMR combines the ability to study and differentiate all phases (solids, gels, and liquids) using a single NMR probe. The general goal of CMP–NMR is to study intact environmental and biological samples to better understand conformation, organization, association, and transfer between and across phases/interfaces that may be lost with conventional sample preparation such as drying or solubilization. To date, all CMP–NMR studies have used 4 mm probes and rotors. Here, a larger 7 mm probehead is introduced which provides ∼3 times the volume and ∼2.4 times the signal over a 4 mm version. This offers two main advantages: (1) the additional biomass reduces experiment time, making 13 C detection at natural abundance more feasible; (2) it allows the analysis of larger samples that cannot fit within a 4 mm rotor. Chicken heart tissue and Hyalella azteca (freshwater shrimp) are used to demonstrate that phase-based spectral editing works with 7 mm rotors and that the additional biomass from the larger volumes allows detection with 13 C at natural abundance. Additionally, a whole pomegranate seed berry (aril) and an intact softgel capsule of hydroxyzine hydrochloride are used to demonstrate the analysis of samples too large to fit inside a conventional 4 mm CMP probe. The 7 mm version introduced here extends the range of applications and sample types that can be studied and is recommended when 4 mm CMP probes cannot provide adequate signal-to-noise (S/N), or intact samples are simply too big for 4 mm rotors.