目的 建立超高效液相色譜串聯(lián)質(zhì)譜（UPLC-MS/MS）法同時(shí)測定茯苓、茯苓皮和茯神中茯苓新酸B、去氫土莫酸、豬苓酸C、去氫茯苓酸和茯苓酸。方法 采用Shim-pack GIST C₁₈ AQ色譜柱（100 mm×2.1 mm，3 μm），以乙腈–0.1%甲酸為流動相，梯度洗脫，體積流量0.4 mL/min，柱溫40 ℃，進(jìn)樣量5 μL。質(zhì)譜采用離子源：ESI，負(fù)離子模式采集，采集模式：多反應(yīng)監(jiān)測（MRM），離子源溫度150 ℃，毛細(xì)管電壓2.5 kV，錐孔電壓40 V，去溶劑氣流量900 L/h，去溶劑氣溫度500 ℃。結(jié)果 茯苓新酸B、去氫土莫酸、豬苓酸C、去氫茯苓酸和茯苓酸在各自的線性范圍內(nèi)線性關(guān)系良好，平均回收率分別為97.80%、99.65%、97.32%、102.82%、99.57%，RSD值分別為3.46%、1.29%、3.01%、3.11%、1.89%。茯苓皮中5種三萜類成分含量均高于茯苓和茯神。結(jié)論 本法具有分析速度快、準(zhǔn)確度高的優(yōu)點(diǎn)，可為茯苓、茯苓皮和茯神的質(zhì)量標(biāo)準(zhǔn)提高和開發(fā)利用提供依據(jù)。

Objective To establish an UPLC-MS/MS method for simultaneous determination of poricoic acid B, dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid, and pachymic acid in Poria, Poria peel, and Poria with hostwood. Methods Shim-pack GIST C₁₈ AQ column (100 mm × 2.1 mm, 3 μm) was used with acetonitrile -0.1% formic acid as the mobile phase by gradient elution. The flow rate was 0.4 mL/min, the column temperature was 40 ℃, and the injection volume was 5 μL. Mass spectrometry adopted the following conditions: ion source: ESI, negative ion mode collection, collection mode: multi-reaction monitoring (MRM), ion source temperature 150 ℃, capillary voltage 2.5 kV, cone voltage 40 V, desolvent gas flow 900 L/h, and desolvent gas temperature 500 ℃. Results Poricoic acid B, dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid, and pachymic acid showed good linear relationship within their linear range. The average recoveries were 97.80%, 99.65%, 97.32%, 102.82%, and 99.57% with RSD values of 3.46%, 1.29%, 3.01%, 3.11%, and 1.89%. The content of five triterpenoids in Poria peel was higher than those in Poria and Poria with hostwood. Conclusion This method has the advantages of fast analysis speed and high accuracy, and can provide a basis for the improvement of the quality standard and the development and utilization of Poria, Poria peel, and Poria with hostwood.

R286.02

陜西省重點(diǎn)研發(fā)計(jì)劃項(xiàng)目（2020SF-090）