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[摘要]
目的 建立半夏及其伪品虎掌南星中水麦冬酸的专属性检测方法。方法 样品经水超声提取,利用高分离度快速液相色谱-三重四极杆质谱(rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry,RRLC-QQQ/MS)检测水麦冬酸。采用Agilent SB-C18(2.1 mm×50 mm,1.8 μm)色谱柱,以乙腈-0.1%甲酸(5∶95)为流动相。柱温30℃,体积流量0.2 mL/min,进样量1 μL。离子化模式为ESI-,选择m/z187→143和m/z187→99作为检测离子对,进行多反应监测。结果 检出限为4.6 μg/L。11批半夏中有3批检出水麦冬酸,7批虎掌南星均检出水麦冬酸,半夏中水麦冬酸含量低于虎掌南星。结论 所建方法专属、准确、快速、简便,可为半夏的质量控制提供参考。
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[Abstract]
Objective To establish a specific identification method of triglochinic acid in Pinelliae Rhizoma and its counterfeit, Pinelliae Pedatisectae Rhizoma. Methods Followedby ultrasonic extraction with water, the samples were analyzed using rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry (RRLC-QQQ/MS). The separation was performed on an Agilent SB-C18 (2.1 mm×50 mm, 1.8 μm) column and the column temperature was set at 30℃. The mobile phase was composed of acetonitrile and 0.1% formic acid (5:95) at a flow rate of 0.2 mL/min. The injection volume was 1 μL. Electrospray ionization source was used with negative ion mode and multiple reaction monitoring (MRM) mode was performed with the transitions of m/z187→143 and m/z187→99. Results The limit of detection was 4.6 μg/L. Triglochinic acid was found in 3 out of 11 batches of Pinelliae Rhizoma samples while in all Pinelliae Pedatisectae Rhizoma samples (7 batches). Content of triglochinic acid in Pinelliae Rhizoma was lower than that in Pinelliae Pedatisectae Rhizoma. Conclusion The proposed method was specific, accurate, rapid and simple, which provided reference for quality control of Pinelliae Rhizoma.
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[基金项目]
国家自然科学基金(81303194);国家中医药管理局中药标准化建设项目(ZYBZH-C-JS-32);中国食品药品检定研究院学科带头人培养基金(2017X1)