UHPLC-Q-Exactive-Obitriap MS快速定量附子理中汤10种化学成分  

UHPLC-Q-Exactive-Obitriap MS for quantification of ten components in Fuzi Lizhong Decoction

作　　者：杨阳[1] 辛杨[1,2] 马凤延[1] 王哲[1] 徐蕾[1] 张伟光 马舒伟[3] YANG Yang;XIN Yang;MA Feng-yan;WANG Zhe;XU Lei;ZHANG Wei-guang;MA Shu-wei(College of Chemistry and Chemical Engineering,Qiqihar University,Qiqihar 161006,China;Heilongjiang Key Laboratory of Catalytic Synthesis for Fine Chemicals,Qiqihar University,Qiqihar 161006,China;School of Chinese Materia Medica,Zhejiang Pharmaceutical College,Ningbo 315100,China)

机构地区：[1]齐齐哈尔大学化学与化学工程学院,黑龙江齐齐哈尔161006 [2]齐齐哈尔大学黑龙江省精细化工催化合成重点实验室,黑龙江齐齐哈尔161006 [3]浙江医药高等专科学校中药学院,浙江宁波315100

出　　处：《中草药》2020年第7期1839-1844,共6页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金资助项目(81403067);黑龙江省省属高等学校基本科研业务费科研项目(135209306);浙江省教育厅项目(Y201534599);浙江医药高等专科学校校级重点课题资助项目(ZPCSR2015015)。

摘　　要：目的建立一种同时定量分析附子理中汤中10种化学成分的方法。方法采用超高效液相色谱-质谱(UHPLC-Q-Exactive Obitriap MS)检测,分别对液相色谱流动相、柱温、梯度洗脱条件,质谱分辨率、喷雾电压等条件进行优化,确定附子理中汤10种化学成分同时被检测的液相条件为Hypersil Gold C18色谱柱(50 mm×2.1 mm,1.9μm);柱温30℃;流动相甲醇(A)-水(B),梯度洗脱:0~6 min,25%~80%A,6~7 min,80%~95%A,7~8 min,95%~100%A,8~9 min,100%A;体积流量0.3 mL/min。质谱条件为电喷雾离子源;Targeted-SIM正、负同时分时间段扫描;扫描范围:m/z 200~700(正)、200~500(负);分辨率17 500;毛细管温度300℃;喷雾电压4.0 kV、-3.5 kV;鞘气体积流量35 L/h;S-lens电压50 V。结果定量检测的10种化合物均获得令人满意的线性,r2均大于0.995,其中正离子模式扫描得苯甲酰乌头原碱、苯甲酰新乌头原碱、白术内酯I、白术内酯Ⅱ、党参炔苷含量分别为2.52、0.11、0.46、1.75、5.8μg/mL,负离子模式扫描得大黄素、甘草苷、甘草素、8-姜酚、10-姜酚含量分别为0.35、2.52、0.98、6.65、2.71μg/mL。结论所建立的液相色谱-质谱检测方法快速、检测限低,可为附子理中汤的质量控制及相关化合物的定量分析提供方法学依据。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.

关 键 词：附子理中汤 超高效液相色谱-四级杆轨道阱质谱 定量分析 大黄素 甘草苷 甘草素 

分 类 号：R284.2[医药卫生—中药学]