目的 建立半夏及其偽品虎掌南星中水麥冬酸的專屬性檢測方法。方法 樣品經(jīng)水超聲提取，利用高分離度快速液相色譜-三重四極桿質(zhì)譜（rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry，RRLC-QQQ/MS）檢測水麥冬酸。采用Agilent SB-C₁₈（2.1 mm×50 mm，1.8 μm）色譜柱，以乙腈-0.1%甲酸（5∶95）為流動相。柱溫30℃，體積流量0.2 mL/min，進樣量1 μL。離子化模式為ESI^-，選擇m/z187→143和m/z187→99作為檢測離子對，進行多反應監(jiān)測。結(jié)果 檢出限為4.6 μg/L。11批半夏中有3批檢出水麥冬酸，7批虎掌南星均檢出水麥冬酸，半夏中水麥冬酸含量低于虎掌南星。結(jié)論 所建方法專屬、準確、快速、簡便，可為半夏的質(zhì)量控制提供參考。

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.

國家自然科學基金（81303194）；國家中醫(yī)藥管理局中藥標準化建設(shè)項目（ZYBZH-C-JS-32）；中國食品藥品檢定研究院學科帶頭人培養(yǎng)基金（2017X1）