| 韩丙军，林靖凌，张月，李建国.超声提取和气相色谱-质谱联用测定
猪屎豆种子中“百合碱含量[J].广东农业科学,2014,41(8):131-133 |
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超声提取和气相色谱-质谱联用测定
猪屎豆种子中“百合碱含量 |
| Ultrasonic extraction and determination by GC-MSof monocrotaline in Crotalaria pallida seed |
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| DOI： |
| 中文关键词: 猪屎豆种子 “百合碱 超声提取 气相色谱-质谱联用 |
| 英文关键词: Crotalaria pallida seed monocrotaline ultrasonicextraction gaschromatography-massspectrometry(GC-MS) |
| 基金项目:海南省自然科学基金(809026) |
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| 中文摘要: |
| 采用超声提取方法对猪屎豆种子中的“百合碱进行提取，并使用气相色谱-质谱法测定“百合碱的含
量。超声提取的最佳提取条件为提取温度75益、提取时间60 min、提取功率255 W、料液比25颐1（V颐M）。建立气相色
谱-质谱联用测定“百合碱含量的方法，采用毛细管气相色谱柱DB-5MS (30 m伊0.25 mm伊0.25 滋m)，进样口温度
250益，离子源为EI 源，电离电压为70 eV，GC-MS 接口温度为280益，离子源温度为220益，采用选择粒子扫描模式，
选择m/z 120 和236 作为定性离子，m/z 120 为定量离子。“百合碱在上机液浓度0.10耀2.00 滋g/mL 与峰面积值线性
关系良好（R2越0.9994），最低检测浓度为0.05 滋g/mL。在试验所选择的3 个样品测定中，平均回收率为96%~112%，
RSD 为3.7%~6.7%。 |
| 英文摘要: |
| Monocrotaline in Crotalaria pallida seed was extracted and determined by ultrasonic extraction and gas
chromatography -mass spectrometry (GC -MS), respectively. Optimal extraction conditions were obtained as follows:
extraction temperature 75, extraction time 60 min, extraction power 255 W, solid-liquid ratio 251(VM). For the GC-MS
determination, separation was performed on DB-5MS column(30 m0.25 mm0.25m), the injector temperature was
250益. The mass spectrometer was operated in electron ionization mode with impact ionization voltage 70 eV, a transfer line
temperature of 280, ion source 220, and selected ion monitoring (SIM) mode. The characteristics ions m/z120 and 236
were used as qualitative ions, and m/z 120 was used as quantitative ion. The proposed method showed excellent linear
correlation coefficient (R20.9994) between the concentration (0.10~2.00g/mL) and peak area, and the LOD was 0.05g/
mL. Precision and recovery tests were made with three samples and the results showed that recoveries was 96%-112%,
RSD was 3.7%-6.7%. |
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