{"title":"溶液中高场和低场核磁共振光谱的稳态自由进动序列:挑战和机遇","authors":"Tiago Bueno Moraes , Flávio Vinícius Crizóstomo Kock , Kahlil Schwanka Salome , Andersson Barison , Andre Simpson , Luiz Alberto Colnago","doi":"10.1016/j.jmro.2022.100090","DOIUrl":null,"url":null,"abstract":"<div><p>The receptivity of NMR spectroscopy is low when compared to other techniques. Historically, increasing the strength of the static magnetic field has been the major approach to increase NMR sensitivity. In recent years several polarization transfer protocols have been used to enhance the signal-to-noise ratio (SNR), although they require special accessories and/or sample preparation. In this paper, we consider both the challenges and opportunities of steady-state free precession (SSFP) pulse sequences as a simple and efficient alternative to enhance SNR, in standard high-resolution and benchtop low-resolution NMR spectrometers. The maximum gain in these sequences is obtained with the shortest time between the pulses (Tp). However, when Tp<T<sub>2</sub>, the SSFP signal contains FID and echo components which lead to phase, intensity, and truncation artifacts on spectra obtained by Fast Fourier transform (FT). Several phase alternation SSFP sequences were used to cancel the echo component and minimize these problems in the FT spectra. Krylov base diagonalization method (KBDM) was used to eliminate the phase and truncation problems in spectra acquired by SSFP pulse sequences and can be a viable alternative to FT. The experiments were performed in high and low resolution (bench top) NMR spectrometers and significant enhancements in SNR of low receptivity nuclei such as <sup>13</sup>C and <sup>15</sup>N could be achieved. The SSFP sequences were also shown to enhance SNR in nuclei with high receptivity such as <sup>19</sup>F and <sup>31</sup>P, in very dilute samples, as is common in environmental and biological samples.</p></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"14 ","pages":"Article 100090"},"PeriodicalIF":2.6240,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"1","resultStr":"{\"title\":\"Steady-State Free Precession sequences for high and low field NMR spectroscopy in solution: Challenges and opportunities\",\"authors\":\"Tiago Bueno Moraes , Flávio Vinícius Crizóstomo Kock , Kahlil Schwanka Salome , Andersson Barison , Andre Simpson , Luiz Alberto Colnago\",\"doi\":\"10.1016/j.jmro.2022.100090\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>The receptivity of NMR spectroscopy is low when compared to other techniques. Historically, increasing the strength of the static magnetic field has been the major approach to increase NMR sensitivity. In recent years several polarization transfer protocols have been used to enhance the signal-to-noise ratio (SNR), although they require special accessories and/or sample preparation. In this paper, we consider both the challenges and opportunities of steady-state free precession (SSFP) pulse sequences as a simple and efficient alternative to enhance SNR, in standard high-resolution and benchtop low-resolution NMR spectrometers. The maximum gain in these sequences is obtained with the shortest time between the pulses (Tp). However, when Tp<T<sub>2</sub>, the SSFP signal contains FID and echo components which lead to phase, intensity, and truncation artifacts on spectra obtained by Fast Fourier transform (FT). Several phase alternation SSFP sequences were used to cancel the echo component and minimize these problems in the FT spectra. Krylov base diagonalization method (KBDM) was used to eliminate the phase and truncation problems in spectra acquired by SSFP pulse sequences and can be a viable alternative to FT. The experiments were performed in high and low resolution (bench top) NMR spectrometers and significant enhancements in SNR of low receptivity nuclei such as <sup>13</sup>C and <sup>15</sup>N could be achieved. The SSFP sequences were also shown to enhance SNR in nuclei with high receptivity such as <sup>19</sup>F and <sup>31</sup>P, in very dilute samples, as is common in environmental and biological samples.</p></div>\",\"PeriodicalId\":365,\"journal\":{\"name\":\"Journal of Magnetic Resonance Open\",\"volume\":\"14 \",\"pages\":\"Article 100090\"},\"PeriodicalIF\":2.6240,\"publicationDate\":\"2023-06-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"1\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Magnetic Resonance Open\",\"FirstCategoryId\":\"1\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S2666441022000607\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Magnetic Resonance Open","FirstCategoryId":"1","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S2666441022000607","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
Steady-State Free Precession sequences for high and low field NMR spectroscopy in solution: Challenges and opportunities
The receptivity of NMR spectroscopy is low when compared to other techniques. Historically, increasing the strength of the static magnetic field has been the major approach to increase NMR sensitivity. In recent years several polarization transfer protocols have been used to enhance the signal-to-noise ratio (SNR), although they require special accessories and/or sample preparation. In this paper, we consider both the challenges and opportunities of steady-state free precession (SSFP) pulse sequences as a simple and efficient alternative to enhance SNR, in standard high-resolution and benchtop low-resolution NMR spectrometers. The maximum gain in these sequences is obtained with the shortest time between the pulses (Tp). However, when Tp<T2, the SSFP signal contains FID and echo components which lead to phase, intensity, and truncation artifacts on spectra obtained by Fast Fourier transform (FT). Several phase alternation SSFP sequences were used to cancel the echo component and minimize these problems in the FT spectra. Krylov base diagonalization method (KBDM) was used to eliminate the phase and truncation problems in spectra acquired by SSFP pulse sequences and can be a viable alternative to FT. The experiments were performed in high and low resolution (bench top) NMR spectrometers and significant enhancements in SNR of low receptivity nuclei such as 13C and 15N could be achieved. The SSFP sequences were also shown to enhance SNR in nuclei with high receptivity such as 19F and 31P, in very dilute samples, as is common in environmental and biological samples.