UPLC-Q-Exactive四极杆-静电场轨道阱高分辨率质谱法同时测定参芪健胃颗粒中8个成分的含量
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篇名: UPLC-Q-Exactive四极杆-静电场轨道阱高分辨率质谱法同时测定参芪健胃颗粒中8个成分的含量
TITLE: Simultaneous Determination of 8 Components Contents in Shenqi Jianwei Granules by UPLC-Q-Exactive Qua- drupole Electrostatic Field Orbital Hydrazine High Resolution Mass Spectrometry
摘要: 目的:建立同时测定参芪健胃颗粒中绿原酸、芍药苷、橙皮苷、甘草酸铵、柠檬苦素、川陈皮素、橘皮素、党参炔苷含量的方法。方法:采用超高效液相色谱(UPLC)-Q-Exactive四极杆-静电场轨道阱高分辨率质谱法。色谱柱为HypersilGoldC18,流动相为乙腈-0.1%甲酸水溶液(梯度洗脱),流速为0.4mL/min,柱温为35℃,进样量为1μL;采用加热型电喷雾离子源,以正离子检测模式,在质荷比100~1000范围内进行高分辨率全扫描。通过提取目标化合物的精确质量数进行定量,测定2个厂家共3批样品中8个成分的含量。结果:绿原酸、芍药苷、橙皮苷、甘草酸铵、柠檬苦素、川陈皮素、橘皮素、党参炔苷8个成分的检测质量浓度线性范围分别为0.12~1.46、3.51~42.15、2.71~32.55、1.76~21.10、0.04~0.46、0.04~0.24、0.02~0.21、0.01~0.25μg/mL(r≥0.9990);定量限分别为6.06、0.04、0.03、0.02、7.60、0.05、0.02、6.25ng/mL;检测限分别为3.03、0.01、0.01、0.01、3.80、0.01、0.01、2.50ng/mL;精密度、重复性及稳定性(24h)试验的RSD均小于5%(n=6);平均加样回收率为93.16%~97.78%(RSD≤5%,n=6);3批样品中8个成分的含量分别为12.62~13.20、265.01~472.26、234.20~278.90、173.10~255.74、2.32~2.83、2.37~3.58、0.79~1.22、0.91~1.78μg/g。结论:本方法简便、快速、准确且重复性好、灵敏度高,可为参芪健胃颗粒的质量控制提供依据。
ABSTRACT: OBJECTIVE:To develo p a method for simultaneous determination of chlorogenic acid ,paeoniflorin,hesperidin, ammonium glycyrrhizate ,limonin,nobiletin,tangeretin and lobetyolin in Shenqi jianwei granules. METHODS :UPLC-Q-Exactive quadrupole electrostatic field orbital hydrazine high resolution mass spectrometry method was adopted. The determination was performed on Hypersil Gold C 18 column with a mobile phase consisted of acetonile- 0.1% formic acid (gradient elution )at the flow rate of 0.4 mL/min. The column temperature was set at 35 ℃,the sample size was 1 μL. High resolution full scan experiments was performed over the range of m/z 100-1 000 in heating electro-spray lonization and positive mode to extract the accurate mass of analytes. The contents of 8 components were determined in 3 batches of samples from 2 manufacturers. RESULTS :The linear range of chlorogenic acid ,paeoniflorin,hesperidin,ammonium glycyrrhizate ,limonin,nobiletin,tangeretin and lobetyolin were 0.12-1.46,3.51-42.15,2.71-32.55,1.76-21.10,0.04-0.46,0.04-0.24,0.02-0.21 and 0.01-0.25 μg/mL,respectively(all r≥0.999 0). The limits of quantitation were 6.06,0.04,0.03,0.02,7.60,0.05,0.02,6.25 ng/mL,respectively. The limits of detection were 3.03,0.01,0.01,0.01,3.80,0.01,0.01,2.50 ng/mL,respectively. RSDs of precision ,reproducibility and stability (24 h)tests were all lower than 5%(n=6). Average recoveries were 93.16%-97.78%(RSD≤5%,n=6). The contents of 8 components in 3 batches of samples were 12.62-13.20,265.01-472.26,234.20-278.90,173.10-255.74,2.32-2.83,2.37-3.58,0.79-1.22,0.91-1.78 μg/g,respectively. CONCLUSIONS :The established method is simple ,convenient,rapid,accurate,highly reproducible and sensitive,which can be used for quality control of Shenqi jianwei granules.
期刊: 2020年第31卷第05期
作者: 吴丹,刘斌,邹瑜
AUTHORS: WU Dan ,LIU Bin ,ZOU Yu
关键字: 超高效液相色谱-Q-Exactive四极杆-静电场轨道阱高分辨率质谱法;参芪健胃颗粒;含量测定
KEYWORDS: UPLC-Q-Exactive quadrupole electrostatic field orbital hydrazine high resolution mass spectrometry ;Shenqi
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