頁籤選單縮合
題名 | Analysis of Aristolochic Acid in Asarum (Xixin) and Its Preparations by Liquid Chromatography/Tandem Mass Spectrometry=利用LC/MS/MS分析細辛藥材暨其製劑中馬兜鈴酸含量 |
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作者姓名(中文) | 徐雅慧; 羅吉方; 劉芳淑; 林哲輝; | 書刊名 | Journal of Food and Drug Analysis |
卷期 | 17:4 2009.08[民98.08] |
頁次 | 頁274-281+317 |
分類號 | 418.52 |
關鍵詞 | 細辛; 馬兜鈴酸; 細辛濃縮散; 麻黃附子細辛湯; 液相層析串聯式質譜儀; Asarum; Xixin; Aristolochic acid Ⅰ; LC/MS/MS; |
語文 | 英文(English) |
中文摘要 | 本研究建立細辛藥材及其製劑中馬兜鈴酸之 LC/MS/MS分析方法。利用 LC/MS/MS作正離子電灑法 (ESI+) 分析,以 piromidic acid為內部標準品,分離管柱為 C18 (2.1×150 mm),移動相溶媒為 0.1%甲酸 (含 0.1%醋酸氨):乙腈 (65:35, v/v),流速為 0.3 mL/min,選定親代離子與子代離子 (馬兜鈴酸 I之配對離子為 m/z 359及 m/z 298,馬兜鈴酸 II之配對離子為 m/z 329及 m/z 268) 進行多重反應監測 (Multiple Reaction Monitoring) 定量分析。馬兜鈴酸 I與馬兜鈴酸 II儀器檢出極限分別為 2與 2.8 ng/mL。結果顯示細辛檢體均含馬兜鈴酸 I,馬兜鈴酸 II則未檢出。本研究首次探討細辛不同部位中馬兜鈴酸 I分布情形,並比較甲醇抽提物與水抽提物中馬兜鈴酸 I之含量。市售 20件細辛檢體,其根、根莖、葉柄、葉之 75%甲醇抽提物中,馬兜鈴酸 I平均含量分別為 1.23 ± 0.64、1.72 ± 1.38、7.81 ± 4.04、27.13 ± 25.31 ppm;其根、根莖、葉柄、葉之水抽提物中,馬兜鈴酸 I平均含量分別為 0.33 ± 0.32、0.45 ± 0.50、3.98 ± 3.09、6.32 ± 9.75 ppm。結果顯示,馬兜鈴酸 I之含量以葉最高,根最低;水抽提量約為 75%甲醇抽提量之 25-50%。細辛濃縮散 6件與麻黃附子細辛湯 6件中,馬兜鈴酸 I含量範圍分別為 0.35-2.07 ppm與 0.21-1.00 ppm。此項研究結果可供行政部門管理細辛藥材暨其製劑之參考。 |
英文摘要 | A method for analysis of aristolochic acids (AAs: AA-I, AA-II) in Asarum (Xixin, named in Chinese) and its preparations by liquid chromatography coupled with tandem mass spectrometry has been developed. The chromatographic analysis was carried out using a C18 column (2.1×150 mm) and a mixture of 0.1% formic acid (containing 0.1% ammonium acetate) and acetonitrile (65:35, v/v) as the mobile phase at a flow rate of 0.3 mL/min. Piromidic acid was used as an internal standard. The mass detection was measured as the positive ion electrospray ionization mode. The precursor and daughter ions for quantitation were m/z 359 and 298 for AA-I, m/z 329 and 268 for AA-II. The instrument detection limit of AA-I and AA-II was 2 and 2.8 ng/mL, respectively. The result showed that Asarum contained AA-I while AA-II was not detected. AA-I distribution in different parts of Asarum was examined in detail and AA-I content in both methanol and water extracts was also compared in this study. In our twenty samples of Asarum, the average amounts of AA-I in 75% methanol extracts of roots, rhizomes, petioles and leaves were 1.23 ± 0.64, 1.72 ± 1.38, 7.81 ± 4.04 and 27.13 ± 25.31 ppm, respectively. The average amounts of AA-I in water extracts of roots, rhizomes, petioles and leaves were 0.33 ± 0.32, 0.45 ± 0.50, 3.98 ± 3.09 and 6.32 ± 9.75 ppm, respectively. The results indicated that the amounts of AA-I in roots were less than those in petioles and leaves, and the amounts of AA-I in water extracts were about 25 to 50 percent of those in 75% methanol extracts. For Asarum preparations, the amounts of AA-I in each six of Xi-xin-extract-powder and Ma-Huang-Fu-Zi-Xi-Xin-Tang ranged between 0.35-2.07 ppm and 0.21-1.00 ppm, respectively. Results of this study could be provided for the regulatory authority as references. |
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