UPLC-MS/MS法同时测定藿香正气软胶囊中10种成分的含量  

Simultaneous determination of 10 constituents in Huoxiang zhengqi soft capsules by UPLC-MS/MS

作　　者：张强[1] 张纯刚 郭勇 程岚[1] ZHANG Qiang;ZHANG Chungang;GUO Yong;CHENG Lan(College of Pharmacy,Liaoning University of Traditional Chinese Medicine,Liaoning Dalian 116620,China;Shineway Pharmaceutical Group Co.,Ltd.,Shijiazhuang 051430,China)

机构地区：[1]辽宁中医药大学药学院,辽宁大连116620 [2]神威药业集团有限公司,石家庄051430

出　　处：《中国药房》2022年第3期287-292,共6页China Pharmacy

基　　金：国家重点研发计划项目(No.2018YFC1706903)。

摘　　要：目的建立同时测定藿香正气软胶囊中甘草苷、柚皮苷、橙皮苷、新橙皮苷、川陈皮素、白术内酯Ⅲ、欧前胡素、和厚朴酚、异欧前胡素、厚朴酚10种成分含量的超高效液相色谱-串联质谱法。方法 12批藿香正气软胶囊内容物经乙醇超声提取,以Ultimate XB-C18为色谱柱、乙腈-0.1%甲酸溶液为流动相进行梯度洗脱,流速为0.4 mL/min,柱温为30℃;采用电喷雾离子源、正负离子扫描的多反应监测模式。结果甘草苷、柚皮苷、橙皮苷、新橙皮苷、川陈皮素、白术内酯Ⅲ、欧前胡素、和厚朴酚、异欧前胡素、厚朴酚的检测质量浓度线性范围分别为1.64~52.40、1.73~55.20、1.54~49.20、1.71~54.80、1.74~55.60、4.19~134.00、1.51~48.40、1.61~51.60、1.80~57.60、1.74~55.60 ng/mL(r≥0.999 5);定量限分别为0.41、0.43、0.19、0.43、0.11、1.05、0.19、0.40、0.45、0.11ng/mL;精密度、稳定性(24 h)、重复性试验的RSD均小于6%;平均加样回收率分别为102.42%、98.65%、98.34%、101.48%、96.74%、100.40%、104.92%、98.53%、99.50%、105.40%(RSD为1.34%~5.44%,n=9)。12批藿香正气软胶囊中上述10种成分的含量分别为201.21~287.89、5.03~20.37、1 465.56~1 988.35、5.35~9.01、217.09~306.44、1.91~16.17、1 081.59~1 377.12、2 388.34~2 915.13、341.26~397.45、7 633.47~8 976.99μg/g。结论所建含量测定方法便捷、灵敏、准确,可用于藿香正气相关制剂的质量控制与评价。OBJECTIVE To establish the ultra-high performance liquid chromatography-mass spectrometry/mass spectrometry method for simultaneous determination of liquiritin, naringin, hesperidin, neohesperidin, nobiletin, atractylenolide Ⅲ,imperatorin,honokiol,isoimperatorin and magnolol in Huoxiang zhengqi soft capsules. METHODS Twelve batches of Huoxiang zhengqi soft capsules were extracted by ultrasonic extraction with ethanol. The determination was performed on Ultimate XB-C18 column with mobile phase consisted of acetonitrile-0.1% formic acid solution for gradient elution at the flow rate of 0.4 m L/min.The column temperature was 30 ℃. The electrospray ionization source was applied to carry out the positive and negative ion scanning with multiple reaction monitoring mode. RESULTS The linear range of liquiritin,naringin,hesperidin,neohesperidin,nobiletin,atractylenolide Ⅲ, imperatorin, honokiol, isoimperatorin and magnolol were 1.64-52.40,1.73-55.20, 1.54-49.20,1.71-54.80,1.74-55.60,4.19-134.00,1.51-48.40,1.61-51.60,1.80-57.60,1.74-55.60 ng/mL(r≥0.999 5),respectively. The limits of quantitation were 0.41,0.43,0.19,0.43,0.11,1.05,0.19,0.40,0.45,0.11 ng/mL,respectively. RSDs of precision,stability(24 h)and repeatability tests were all lower than 6%. Average recoveries were 102.42%,98.65%,98.34%,101.48%,96.74%,100.40%,104.92%,98.53%,99.50%,105.40%(RSD=1.34%-5.44%,n=9). The contents of the above 10 constituents in 12 batches of Huoxiang zhengqi soft capsules were 201.21-287.89,5.03-20.37,1 465.56-1 988.35,5.35-9.01,217.09-306.44,1.91-16.17,1 081.59-1 377.12,2 388.34-2 915.13,341.26-397.45 and 7 633.47-8 976.99 μg/g,respectively. CONCLUSIONS The established method for content determination is convenient,sensitive and accurate,which can be used for the quality control and evaluation of Huoxiang zhengqi related preparations.

关 键 词：藿香正气软胶囊 超高效液相色谱-串联质谱法 化学成分 质量控制 

分 类 号：R917[医药卫生—药物分析学] R284.1[医药卫生—药学]