目的 建立一種同時(shí)定量分析附子理中湯中10種化學(xué)成分的方法。方法 采用超高效液相色譜-質(zhì)譜（UHPLC-Q-Exactive Obitriap MS）檢測(cè)，分別對(duì)液相色譜流動(dòng)相、柱溫、梯度洗脫條件，質(zhì)譜分辨率、噴霧電壓等條件進(jìn)行優(yōu)化，確定附子理中湯10種化學(xué)成分同時(shí)被檢測(cè)的液相條件為Hypersil Gold C₁₈色譜柱（50 mm×2.1 mm，1.9 μm）；柱溫30 ℃；流動(dòng)相甲醇（A）-水（B），梯度洗脫：0～6 min，25%～80% A，6～7 min，80%～95% A，7～8 min，95%～100% A，8～9 min，100% A；體積流量0.3 mL/min。質(zhì)譜條件為電噴霧離子源；Targeted-SIM正、負(fù)同時(shí)分時(shí)間段掃描；掃描范圍：m/z 200～700（正）、200～500（負(fù)）；分辨率17 500；毛細(xì)管溫度300 ℃；噴霧電壓4.0 kV、-3.5 kV；鞘氣體積流量35 L/h；S-lens電壓50 V。結(jié)果 定量檢測(cè)的10種化合物均獲得令人滿意的線性，r²均大于0.995，其中正離子模式掃描得苯甲酰烏頭原堿、苯甲酰新烏頭原堿、白術(shù)內(nèi)酯I、白術(shù)內(nèi)酯II、黨參炔苷含量分別為2.52、0.11、0.46、1.75、5.8 μg/mL，負(fù)離子模式掃描得大黃素、甘草苷、甘草素、8-姜酚、10-姜酚含量分別為0.35、2.52、0.98、6.65、2.71 μg/mL。結(jié)論 所建立的液相色譜-質(zhì)譜檢測(cè)方法快速、檢測(cè)限低，可為附子理中湯的質(zhì)量控制及相關(guān)化合物的定量分析提供方法學(xué)依據(jù)。

Objective To establish a method for quantifying ten components in Fuzi Lizhong Decoction (FLD). Methods Ultra high performance liquid chromatography-Q-Exactive Obitriap mass spectrometry was used to detect components under optimized conditions as follows:Hypersil Gold C₁₈ column (50 mm×2.1 mm, 1.9 μm), column temperature:30℃, mobile phase:methanol (A)-water (B), gradient elution conditions:0-6 min, 25%-80% A, 6-7 min, 80%-95% A, 7-8 min, 95%-100% A, 8-9 min, 100% A, flow rate:0.3 mL/min; Ion source:electrospray, scan mode:full scan (positive, negative), scan range:m/z 200-700 (positive), 200-500 (negative), resolution:17 500, capillary temperature:300℃, spray voltage:+4.0 kV, -3.5 kV, sheath gas flow rate:35 L/h, S-lens voltage:50 V. Results Satisfactory linearity with correlation coefficient (r²) higher than 0.995 was achieved for each compound. The content of benzoyl aconitine, benzoylmesaconine, atractylenolide I, atractylenolide II and lobetyolin scanned under positive mode in FLD was 2.52, 0.11, 0.46, 1.75 and 5.8 μg/mL respectively, and that of emodin, glycyrrhizin, liguiritigenin, 8-gingerol, 10-gingerol scanned under negative mode in FLD was 0.35, 2.52, 0.98, 6.65 and 2.71 μg/mL, respectively. Conclusion The developed liquid chromatography-mass spectrometry method was fastwith low limit of detection, which could provide methodological basis for quality control of FLD as well as quantification of these compounds.

國家自然科學(xué)基金資助項(xiàng)目（81403067）；黑龍江省省屬高等學(xué)?；究蒲袠I(yè)務(wù)費(fèi)科研項(xiàng)目（135209306）；浙江省教育廳項(xiàng)目（Y201534599）；浙江醫(yī)藥高等?？茖W(xué)校校級(jí)重點(diǎn)課題資助項(xiàng)目（ZPCSR2015015）