目的 建立HPLC梯度洗脫法同時測定仲景胃靈丸中茴香醛、肉桂醇、肉桂酸、桂皮醛、延胡索乙素、去氫紫堇堿、紫堇堿和四氫小檗堿，并采用化學(xué)計(jì)量學(xué)方法對其結(jié)果進(jìn)行分析評價(jià)。方法 采用HPLC法，Agilent Zorbax SB C₁₈色譜柱（250 mm×4.6 mm，5μm），柱溫30 ℃；乙腈–0.1%冰醋酸水溶液為流動相，梯度洗脫，體積流量0.9 mL/min；進(jìn)樣量10 μL；檢測波長分別為248 nm（檢測茴香醛）、280 nm（檢測肉桂醇、肉桂酸、桂皮醛、延胡索乙素、去氫紫堇堿、紫堇堿和四氫小檗堿）。采用統(tǒng)計(jì)軟件對仲景胃靈丸中8種成分的質(zhì)量分?jǐn)?shù)進(jìn)行化學(xué)計(jì)量學(xué)評價(jià)。結(jié)果 茴香醛、肉桂醇、肉桂酸、桂皮醛、延胡索乙素、去氫紫堇堿、紫堇堿、四氫小檗堿分別在0.96～24.00、1.78～44.50、20.06～501.50、3.92～98.00、2.89～72.25、2.13～53.25、1.36～34.00、0.59～14.75μg/mL線性關(guān)系良好；平均加樣回收率分別為96.97%、97.81%、100.04%、99.13%、98.91%、96.89%、97.58%、98.34%，RSD值分別為1.04%、1.51%、0.54%、1.01%、0.92%、1.32%、1.36%、1.41%?；瘜W(xué)計(jì)量學(xué)表明10批仲景胃靈丸聚為3類，主成分1～4是影響仲景胃靈丸整體質(zhì)量的主要因子。結(jié)論 以茴香醛、肉桂醇、肉桂酸、桂皮醛、延胡索乙素、去氫紫堇堿、紫堇堿、四氫小檗堿同步測定的HPLC法和化學(xué)計(jì)量學(xué)方法可用于仲景胃靈丸多指標(biāo)質(zhì)量評價(jià)。

Objective To establish an HPLC gradient elution method for simultaneous determination of 4-methoxybenzaldehyde, cinnamyl alcohol, cinnamic acid, cinnamaldehyde, tetrahydropalmatine, dehydrocorydalin, corydaline, and tetrahydroberberine in Zhongjing Weiling Pills, and the results was analyzed by chemometrics method.Methods The HPLC method was used on Agilent Zorbax SB C₁₈ column (250 mm×4.6 mm, 5 μm), and the column temperature was set at 30 ℃. The mobile phase was consisted of acetonitrile and water containing 0.1% glacial acetic acid aqueous solution in gradient elution, and the flow rate was set at 0.9 mL/min. The detection wavelengths were set at 248 nm for 4-methoxybenzaldehyde and 280 nm for cinnamyl alcohol, cinnamic acid, cinnamaldehyde, tetrahydropalmatine, dehydrocorydalin, corydaline, and tetrahydroberberine. The chemometrics evaluation was conducted for the content results of eight constituents in Zhongjing Weiling Pills by Statistical Software.Results There were good linear relationships for4-methoxybenzaldehyde, cinnamyl alcohol, cinnamic acid, cinnamaldehyde, tetrahydropalmatine, dehydrocorydalin, corydaline, and tetrahydroberberine within the ranges of 0.96 — 24.00, 1.78 — 44.50, 20.06 — 501.50, 3.92 — 98.00, 2.89 — 72.25, 2.13 — 53.25, 1.36 — 34.00, and 0.59 — 14.75 μg/mL. Those average recoveries were 96.97%, 97.81%, 100.04%, 99.13%, 98.91%, 96.89%, 97.58%, and 98.34% with the RSD values of 1.04%, 1.51%, 0.54%, 1.01%, 0.92%, 1.32%, 1.36%, and 1.41%, respectively. The chemometrics method showed that the 10 batches of Zhongjing Weiling Pills were divided into three categories. The 1 — 4 principal components were the main factor affecting the quality of Zhongjing Weiling Pills.Conclusion Simultaneous determination of 4-methoxybenzaldehyde, cinnamyl alcohol, cinnamic acid, cinnamaldehyde, tetrahydropalmatine, dehydrocorydalin, corydaline, and tetrahydroberberine by HPLC and chemometrics method can be used to evaluate the quality of Zhongjing Weiling Pills.

R284.1

河南省科技攻關(guān)項(xiàng)目（182102310096）