目的 采用超高效液相色谱-单四极杆质谱（ultra-high performance liquid chromatography-quadrupole-mass spectrometry，UHPLC-Q-MS）法，建立宣肺败毒颗粒（Xuanfei Baidu Granules，XBG）中14个成分的含量测定方法。方法 采用Waters HSS T3色谱柱（100 mm×2.1 mm，1.8 μm）；以0.05%甲酸水溶液-乙腈为流动相梯度洗脱，体积流量0.4 mL/min；柱温40 ℃；进样量2 μL；采用电喷雾电离源（electrospray ionization，ESI）质谱，扫描方式为选择离子监测（selected ion monitoring，SIM）模式。结果 在48 min内实现了XBG中14种成分（麻黄碱、L-苦杏仁苷、苦杏仁苷、槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷、戟叶马鞭草苷、马鞭草苷、虎杖苷、甘草苷、类叶升麻苷、异类叶升麻苷、异绿原酸A、柚皮苷、野漆树苷和甘草酸）的分离和含量测定，14种成分在各自的质量浓度范围内均有良好的线性关系（r≥0.993 1），定量限为1.779～52.010 ng/mL，平均加样回收率为92.9%～106.3%，RSD为0.7%～5.5%。10个批次XBG中14种成分的含量测定结果表明，XBG的批次间一致性较好。结论 所建立的UHPLC-Q-MS分析方法专属性强，准确度高，可为XBG的质量控制以及临床应用提供参考。

Objective To establish an ultra-high performance liquid chromatography-quadrupole-mass spectrometry (UHPLC-Q-MS) method for the simultaneous determination of 14 constituents in Xuanfei Baidu Granules (XBG). Methods The separation was performed on a Waters HSS T3 column (100 mm×2.1 mm, 1.8 μm) by using a gradient elution with a mobile phase consisting of water containing 0.05% formic acid-acetonitrile at a flow rate of 0.4 mL/min. The column temperature was 40 ℃, and the injection volume was 2 μL. The mass spectrometry was equipped with electrospray ionization (ESI) source and performed in selected ion monitoring (SIM) mode. Results The separation and determination of 14 constituents (ephedrine, L-amygdalin, amygdalin, quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside, hastatoside, verbenalin, polydatin, liquiritin, acteoside, isoacteoside, isochlorogenic acid A, naringin, rhoifolin, and glycyrrhizic acid) in XBG were achieved within 48 min. Good linear relationships (r ≥ 0.993 1) were obtained for all 14 constituents within their mass concentration ranges. The average recovery rates were 92.9%—106.3%, RSDs were 0.7%—5.5%. The limits of quantification were 1.779—52.010 ng/mL. The determination results of 14 constituents in 10 batches of XBG demonstrated good consistency among different batches of XBG. Conclusion The established method shows good specificity and accuracy. The results provide references for the quality control and clinical application of XBG.

R283.6

国家重点研发计划——战略性科技创新合作专项(2021YFE0200300)