UPLC-MS/MS 法测定七神益气滴丸中的四种化学成分

IF 0.6 4区 医学 Q4 CHEMISTRY, MEDICINAL
Qin Lili, Honglian Zhang, Yanxia Wang, Yingying Liang, Li Qiang, Xuerong Xie
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The column temperature was 40℃, the injection volume was 3 µL, and the flow rate was 0.2 mL⋅min–1. Finally, the determination method was built to test four chemical constituents under the multiple reaction monitoring (MRM) analysis mode. The retention times of protocatechuic acid, salvianolic acid B, rosmarinic acid, and cryptotanshinone were 1.26, 1.32, 1.35, and 6.76 min, respectively. In addition, the concentration ranges of four compounds were 0.25–2.0 µg⋅mL–1, 10.0–50.0 µg⋅mL–1, 5.0–50.0 µg⋅mL–1, and 1.0–10.0 µg⋅mL–1, respectively. And the standard curve showed a good linear relationship in a reasonable range ( r2 ≥ 0.9950). The average recovery rate was from 96% to 124%. The contents of protocatechuic acid, salvianolic acid B, rosmarinic acid, and cryptotanshinone were 0.12%–0.022%, 17%–8.4%, and 6.5%–8.6% in seven batches of Qishen Yiqi dripping pills, which were in the range of 23%–31%. 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引用次数: 0

摘要

本研究建立了超高效液相色谱-质谱联用(UPLC-MS/MS)法测定芪肾益气滴丸中原儿茶酸(C7H6O4)、丹酚酸B (C36H30O16)、迷迭香酸(C19H14O3)、隐丹参酮(C19H20O3)的含量。按一定的料液比选择甲醇作为溶剂作为溶液,采用超声波提取法制备样品溶液。采用UPLC-MS/MS对芪肾益气滴丸的含量进行定量分析。然后,色谱条件如下:固定相为Agilent ZORBAX SB-C18 (2.1 mm × 100 mm, 1.8µm),流动相为乙腈- 0.1%甲酸水。柱温40℃,进样量3µL,流速0.2 mL⋅min-1。最后,在多重反应监测(MRM)分析模式下,建立检测四种化学成分的测定方法。原儿茶酸、丹酚酸B、迷迭香酸和隐丹参酮的保留时间分别为1.26、1.32、1.35和6.76 min。4种化合物的浓度范围分别为0.25 ~ 2.0µg⋅mL-1、10.0 ~ 50.0µg⋅mL-1、5.0 ~ 50.0µg⋅mL-1和1.0 ~ 10.0µg⋅mL-1。标准曲线在合理范围内呈良好的线性关系(r2≥0.9950)。平均回收率为96% ~ 124%。七批芪肾益气滴丸中原儿茶酸、丹酚酸B、迷迭香酸、隐丹参酮的含量分别为0.12% ~ 0.022%、17% ~ 8.4%、6.5% ~ 8.6%,含量范围为23% ~ 31%。仪器运行稳定,方法准确度和重复性好(相对标准偏差[RSD]≤3%)。10 h内检测结果稳定。不同批次的四种成分含量不同。建立气肾益气滴丸中4种化学成分的定量测定方法,为体内质量评价提供参考。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Determination of Four Chemical Components in Qishen Yiqi Dripping Pills by UPLC-MS/MS Method
In this study, the ultrahigh performance liquid chromatography mass spectrometry/mass spectrometry (UPLC-MS/MS) method was established to test the contents of protocatechuic acid (C7H6O4), salvianolic acid B (C36H30O16), rosmarinic acid (C19H14O3), and cryptotanshinone (C19H20O3) in Qishen Yiqi dripping pills. Methanol was chosen as the solvent according to a certain material–liquid ratio as a solution, and the ultrasonic extraction method was used to prepare the sample solution. UPLC-MS/MS was used to complete a quantitative analysis of the contents of Qishen Yiqi dripping pills. Then, the chromatographic conditions were shown as follows. The stationary phase was Agilent ZORBAX SB-C18 (2.1 mm × 100 mm, 1.8 µm), and the mobile phase was acetonitrile–0.1% formic acid water. The column temperature was 40℃, the injection volume was 3 µL, and the flow rate was 0.2 mL⋅min–1. Finally, the determination method was built to test four chemical constituents under the multiple reaction monitoring (MRM) analysis mode. The retention times of protocatechuic acid, salvianolic acid B, rosmarinic acid, and cryptotanshinone were 1.26, 1.32, 1.35, and 6.76 min, respectively. In addition, the concentration ranges of four compounds were 0.25–2.0 µg⋅mL–1, 10.0–50.0 µg⋅mL–1, 5.0–50.0 µg⋅mL–1, and 1.0–10.0 µg⋅mL–1, respectively. And the standard curve showed a good linear relationship in a reasonable range ( r2 ≥ 0.9950). The average recovery rate was from 96% to 124%. The contents of protocatechuic acid, salvianolic acid B, rosmarinic acid, and cryptotanshinone were 0.12%–0.022%, 17%–8.4%, and 6.5%–8.6% in seven batches of Qishen Yiqi dripping pills, which were in the range of 23%–31%. The instrument ran stably, and the method had good accuracy and repeatability (relative standard deviation [RSD] ≤ 3%). Additionally, the test result was stable within 10 h. The contents of the four constituents were different among different batches. The quantitative method was established to determine the four chemical components in Qishen Yiqi dripping pills, which could provide a reference for quality evaluation in vivo.
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来源期刊
Pharmacognosy Magazine
Pharmacognosy Magazine CHEMISTRY, MEDICINAL-
CiteScore
1.87
自引率
0.00%
发文量
37
审稿时长
3 months
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