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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 |
| 阅读数： | 416 次 |
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