Detection of 6-(Methylsulfinyl)hexyl Isothiocyanate (6-MITC) and Its Conjugate with N-Acetyl-L-cysteine (NAC) by High Performance Liquid Chromatograpy-Atmospheric Pressure Chemical Ionization Mass Spectrometry (HPLC-MS/APCI)
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- Yamaguchi Hideaki
- Department of Clinical Pharmacy, Faculty of Pharmaceutical Sciences, Aomori University
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- Noshita Toshiro
- Department of Clinical Pharmacy, Faculty of Pharmaceutical Sciences, Aomori University
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- Kidachi Yumi
- Department of Clinical Pharmacy, Faculty of Pharmaceutical Sciences, Aomori University
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- Umetsu Hironori
- Department of Life Sciences, Junior Collage, Gifu Shotoku Gakuen University
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- Fuke Yoko
- Department of Food Science and Human Nutrition, Tokyo Metropolitan University
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- Ryoyama Kazuo
- Department of Clinical Pharmacy, Faculty of Pharmaceutical Sciences, Aomori University
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A method using high-performance liquid chromatography (HPLC) and atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) was established for the detection of 6-(methylsulfinyl)hexyl isothiocyanate (6-MITC) and its conjugate with N-acetyl-L-cysteine (NAC). The optimal chromatographic conditions were obtained on an ODS column (150×4.6 mm, 3 μm) with the column temperature at 37 °C. The mobile phase consisted of a methanol-0.1% trifluoroacetic acid (TFA) mixture (50 : 50, v/v), and the flow rate was 0.3 ml/min. The detection wavelength was set at 220 nm. The identities of the peaks were accomplished by comparing retention times (tR), UV and mass data. All calibration curves showed good linear regression (correlation coefficients for 6-MITC and NAC>0.999) within test ranges. The developed method provided satisfactory precision calculated as percent coefficient of variation with overall intra-day and inter-day variations of less than 5% (4.1 and 4.9% for 6-MITC; 4.2 and 4.9% for NAC). Both 6-MITC and NAC had good responses in the positive APCI and formed strong [M+H]+ ions in the full scan spectra at an m/z of 206 and 164, respectively. The presence of the [M+H]+ ion for the 6-MITC/NAC conjugate was also observed at an m/z of 369. To our best knowledge, this is the first report that describes the formation of the 6-MITC/NAC conjugate and its detection method by HPLC-MS.
収録刊行物
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- ＣＨＥＭＩＣＡＬ ＆ ＰＨＡＲＭＡＣＥＵＴＩＣＡＬ ＢＵＬＬＥＴＩＮ
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ＣＨＥＭＩＣＡＬ ＆ ＰＨＡＲＭＡＣＥＵＴＩＣＡＬ ＢＵＬＬＥＴＩＮ 56 (5), 715-719, 2008
公益社団法人 日本薬学会
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詳細情報 詳細情報について
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- CRID
- 1390001204171094400
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- NII論文ID
- 110006663999
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- NII書誌ID
- AA00602100
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- ISSN
- 13475223
- 00092363
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- NDL書誌ID
- 9473898
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- 本文言語コード
- en
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- データソース種別
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- JaLC
- NDL
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