PMC:7594251 / 23879-26942
Annnotations
{"target":"https://pubannotation.org/docs/sourcedb/PMC/sourceid/7594251","sourcedb":"PMC","sourceid":"7594251","source_url":"https://www.ncbi.nlm.nih.gov/pmc/7594251","text":"2.2.2. 2D 1H,1H-TOCSY\nTotal Correlation Spectroscopy (TOCSY) also originally known as the Homonuclear Hartmann Hahn (HOHAHA) experiment can be considered an extension of the 2D 1H,1H-COSY experiment. The difference between the two experiments is that a TOCSY experiment will show multiple cross-peaks including indirectly coupled nuclei (i.e., longer range via scalar coupling) throughout the J-coupled spin system of a chemical compound. The basic pulse sequence of the TOCSY consists of excitation by a 90° pulse, followed by a free variable evolution period which encodes the indirect dimension. This is normally followed by an isotropic mixing sequence to transfer magnetization between spins via the strong scalar coupling. The mixing generates in-phase magnetization throughout a spin coupled network of the associated nuclei during the mixing time. Lastly, a direct detection is performed. A major advantage of the TOCSY experiment is that it detects in-phase magnetization (i.e., pure absorptive line-shape) which is far easier to analyze compared to the anti-phase information in the phase sensitivity COSY-type experiment. The isotropic mixing is usually performed using a composite pulse scheme such as WALTZ, MLEV or DIPSI [133,134] pulse train, and can be sandwiched between two z-filters [135] where isotropic mixing is performed on the longitudinal magnetization. The most obvious advantage of TOCSY is that all cross-peaks of the same spin system can be observed for whole spin system at once. This is useful for identifying the complete network of spins and reducing the ambiguity of any spectral overlap. The TOCSY experiment can be produced as 1D with a relatively shorter time and easier analysis compared to 2D but lacks the benefit of multi-dimensional resolution. The 2D TOCSY is usually done to resolve spectra overlap [50] when first identifying molecules [136,137,138]. For example, Jiang et al. used this to predict the response to gemcitabine-carboplatin (GC) chemotherapy in patients with metastatic breast cancer who were previously exposed to treatment with both anthracyclines and taxanes [137]. For that, researchers collected serum samples from 29 patients prior to treatment and measured them using 1D 1H-NMR. Additionally, they conducted 2D NMR experiments such as the 1H,1H-COSY, 1,1H-TOCSY, 1H,13C-HSQC, and 1H,13C-HMBC to help assign serum metabolites. After receiving the treatment with gemcitabine-carboplatin, patients were divided into four groups based on the results from the computed tomography: complete response (CR), partial response (PR), stable disease (SD), or progressive disease (PD). After comparing NMR results prior to the treatment with the outcome of chemotherapy, the researchers observed lower baseline levels of serum format and acetate in breast cancer patients who progressed with the disease than in those who achieved a clinical benefit from therapy, indicating that those two biomarkers could be used to distinguish between patients who will benefit from GC treatment from those who do not 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