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Determination and analysis of ustiloxins A and B by LC-ESI-MS and HPLC in false smut balls of rice.

Shan T, Sun W, Liu H, Gao S, Lu S, Wang M, Sun W, Chen Z, Wang S, Zhou L - Int J Mol Sci (2012)

Bottom Line: Ustiloxins are cyclopeptide mycotoxins produced by the pathogenic fungus Villosiclava virens of rice false smut.Ustiloxins A and B as two main mycotoxins were determined conveniently by LC-ESI-MS in the water extract from rice false smut balls which were mostly composed of the chlamydospores and mycelia of the pathogen.This is the first report on the determination and analysis of ustiloxins A and B simultaneously by LC-ESI-MS and HPLC in false smut balls of rice.

View Article: PubMed Central - PubMed

Affiliation: College of Agronomy and Biotechnology, China Agricultural University, Beijing 100193, China; E-Mails: shan5400388@163.com (T.S.); sunweibo.1001@163.com (W.S.); hardyliuhao@163.com (H.L.); gaoshankonglong@163.com (S.G.); shiqionglu@126.com (S.L.); wangma@cau.edu.cn (M.W.); wxs@cau.edu.cn (W.S.).

ABSTRACT
Ustiloxins are cyclopeptide mycotoxins produced by the pathogenic fungus Villosiclava virens of rice false smut. Ustiloxins A and B as two main mycotoxins were determined conveniently by LC-ESI-MS in the water extract from rice false smut balls which were mostly composed of the chlamydospores and mycelia of the pathogen. Both ustiloxins A and B in the water extract were also quantitatively analyzed by HPLC. This is the first report on the determination and analysis of ustiloxins A and B simultaneously by LC-ESI-MS and HPLC in false smut balls of rice.

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Primary determination of the ustiloxin-like compounds from the water extract of rice false smut balls by LC-ESI-MS. (A) and (B) were the spectra of HPLC-UV and total ion chromatograms, respectively. (C–G) were the ESI-MS spectra of peaks 1, 2, 3, 4 and 5, respectively, appearing in (A) and (B).
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f1-ijms-13-11275: Primary determination of the ustiloxin-like compounds from the water extract of rice false smut balls by LC-ESI-MS. (A) and (B) were the spectra of HPLC-UV and total ion chromatograms, respectively. (C–G) were the ESI-MS spectra of peaks 1, 2, 3, 4 and 5, respectively, appearing in (A) and (B).

Mentions: Figure 1 shows the primary determination of the ustiloxin-like compounds from the water extract of rice false smut balls by LC-ESI-MS. The spectrum with detection wavelength from 190 to 400 nm was employed to obtain more peaks in the HPLC-UV chromatogram. The major detection wavelength of 220 nm was selected. Five peaks (i.e., peaks 1–5) appeared in both HPLC-UV and total ion chromatograms (Figure 1A,B) with retention times of 8.4 min, 13.5 min, 15.4 min, 16.9 min and 24.0 min, respectively. They were selected for further ESI-MS analysis with the results shown in Figure 1. By comparison with the molecular weights of the ustiloxins previously reported [1,10,11], we preliminarily concluded that peaks 1–4 should be ustiloxin-like compounds. At 646.3 m/z (Figure 1C) should be the peak of the [M + H]+ ion of ustiloxin B that corresponds to peak 1 in Figure 1A,B. Similarly, at 559.2 m/z (Figure 1D) should be the peak of the [M + H]+ ion of ustiloxin C that corresponds to peak at 2, 674.3 m/z (Figure 1E) should be the peak of the [M + H]+ ion of ustiloxin A that corresponds to peak 3, and at 495.2 m/z and 517.2 m/z (Figure 1F) should be the peaks of the [M + H]+ and the [M + Na]+ ions of ustiloxin D that correspond to peak 4 in Figure 1A,B. These ustiloxin-like compounds need to be purified and further confirmed by spectroscopic methods such as NMR and MS. According to the peak areas in the HPLC profile (Figure 1A) and the ion relative abundances in the TIC spectrum (Figure 1B), peaks 1, 3 and 5 should correspond to the three main components in the water extract of rice false smut balls. Peak 5 (in Figure 1A,B) with a major ion peak at m/z 587.2 shown in Figure 1G has not been reported previously. It needs to be purified and further confirmed.


Determination and analysis of ustiloxins A and B by LC-ESI-MS and HPLC in false smut balls of rice.

Shan T, Sun W, Liu H, Gao S, Lu S, Wang M, Sun W, Chen Z, Wang S, Zhou L - Int J Mol Sci (2012)

Primary determination of the ustiloxin-like compounds from the water extract of rice false smut balls by LC-ESI-MS. (A) and (B) were the spectra of HPLC-UV and total ion chromatograms, respectively. (C–G) were the ESI-MS spectra of peaks 1, 2, 3, 4 and 5, respectively, appearing in (A) and (B).
© Copyright Policy - open-access
Related In: Results  -  Collection

License 1 - License 2
Show All Figures
getmorefigures.php?uid=PMC3472744&req=5

f1-ijms-13-11275: Primary determination of the ustiloxin-like compounds from the water extract of rice false smut balls by LC-ESI-MS. (A) and (B) were the spectra of HPLC-UV and total ion chromatograms, respectively. (C–G) were the ESI-MS spectra of peaks 1, 2, 3, 4 and 5, respectively, appearing in (A) and (B).
Mentions: Figure 1 shows the primary determination of the ustiloxin-like compounds from the water extract of rice false smut balls by LC-ESI-MS. The spectrum with detection wavelength from 190 to 400 nm was employed to obtain more peaks in the HPLC-UV chromatogram. The major detection wavelength of 220 nm was selected. Five peaks (i.e., peaks 1–5) appeared in both HPLC-UV and total ion chromatograms (Figure 1A,B) with retention times of 8.4 min, 13.5 min, 15.4 min, 16.9 min and 24.0 min, respectively. They were selected for further ESI-MS analysis with the results shown in Figure 1. By comparison with the molecular weights of the ustiloxins previously reported [1,10,11], we preliminarily concluded that peaks 1–4 should be ustiloxin-like compounds. At 646.3 m/z (Figure 1C) should be the peak of the [M + H]+ ion of ustiloxin B that corresponds to peak 1 in Figure 1A,B. Similarly, at 559.2 m/z (Figure 1D) should be the peak of the [M + H]+ ion of ustiloxin C that corresponds to peak at 2, 674.3 m/z (Figure 1E) should be the peak of the [M + H]+ ion of ustiloxin A that corresponds to peak 3, and at 495.2 m/z and 517.2 m/z (Figure 1F) should be the peaks of the [M + H]+ and the [M + Na]+ ions of ustiloxin D that correspond to peak 4 in Figure 1A,B. These ustiloxin-like compounds need to be purified and further confirmed by spectroscopic methods such as NMR and MS. According to the peak areas in the HPLC profile (Figure 1A) and the ion relative abundances in the TIC spectrum (Figure 1B), peaks 1, 3 and 5 should correspond to the three main components in the water extract of rice false smut balls. Peak 5 (in Figure 1A,B) with a major ion peak at m/z 587.2 shown in Figure 1G has not been reported previously. It needs to be purified and further confirmed.

Bottom Line: Ustiloxins are cyclopeptide mycotoxins produced by the pathogenic fungus Villosiclava virens of rice false smut.Ustiloxins A and B as two main mycotoxins were determined conveniently by LC-ESI-MS in the water extract from rice false smut balls which were mostly composed of the chlamydospores and mycelia of the pathogen.This is the first report on the determination and analysis of ustiloxins A and B simultaneously by LC-ESI-MS and HPLC in false smut balls of rice.

View Article: PubMed Central - PubMed

Affiliation: College of Agronomy and Biotechnology, China Agricultural University, Beijing 100193, China; E-Mails: shan5400388@163.com (T.S.); sunweibo.1001@163.com (W.S.); hardyliuhao@163.com (H.L.); gaoshankonglong@163.com (S.G.); shiqionglu@126.com (S.L.); wangma@cau.edu.cn (M.W.); wxs@cau.edu.cn (W.S.).

ABSTRACT
Ustiloxins are cyclopeptide mycotoxins produced by the pathogenic fungus Villosiclava virens of rice false smut. Ustiloxins A and B as two main mycotoxins were determined conveniently by LC-ESI-MS in the water extract from rice false smut balls which were mostly composed of the chlamydospores and mycelia of the pathogen. Both ustiloxins A and B in the water extract were also quantitatively analyzed by HPLC. This is the first report on the determination and analysis of ustiloxins A and B simultaneously by LC-ESI-MS and HPLC in false smut balls of rice.

Show MeSH