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目的:建立同时测定谷红注射液中乙酰谷酰胺,羟基红花黄色素A,芦丁,紫丁香苷,山柰素,山柰酚,槲皮素含量的方法。方法:采用超高效液相色谱-串联质谱法。Phenomenex Kinetex C18色谱柱(2.1 mm×50 mm,5μm),流动相乙腈-0.1%甲酸水溶液,梯度洗脱,流速0.5 m L·min~(-1);质谱采用正负离子同时监测,多反应监测模式(MRM),进样量5μL。结果:谷红注射液中乙酰谷酰胺,羟基红花黄色素A,芦丁,紫丁香苷,山柰素,山柰酚,槲皮素质量浓度线性范围分别在10.36~663.0,0.500 0~32.00,0.047 8~3.059,0.200 0~12.80,0.032 4~2.074,0.675 0~43.20,0.142 5~9.120μg·L~(-1)线性关系良好;平均加样回收率分别为97.0%~99.2%,RSD<3.4%(n=6);7种成分在3批样品中的质量浓度依次为乙酰谷酰胺28.5~32.4 g·L~(-1),羟基红花黄色素A 1.02~1.23 g·L~(-1),芦丁14.3~17.6 mg·L~(-1),紫丁香苷101~123 mg·L~(-1),山柰素12.1~14.9μg·L~(-1),山柰酚0.138~0.155 mg·L~(-1),槲皮素73.4~95.6μg·L~(-1)。结论:该方法简、快速、高效、准确、可靠,适用于同时测定乙酰谷酰胺,羟基红花黄色素A,芦丁,紫丁香苷,山柰素,山柰酚,槲皮素7种有效成分,为该制剂建立更全面的质量控制方法提供依据。
Objective: To establish a method for the simultaneous determination of acetylglutamine, hydroxysafflor yellow A, rutin, syringin, kaempferol, kaempferol and quercetin in Guhong injection. Methods: Using ultra performance liquid chromatography-tandem mass spectrometry. Phenomenex Kinetex C18 column (2.1 mm × 50 mm, 5 μm) was used. The mobile phase was acetonitrile-0.1% formic acid aqueous solution with gradient elution at a flow rate of 0.5 mL · min -1. Mode (MRM), injection volume 5μL. Results: The linear ranges of glutamic oxalate, hydroxysafflor yellow A, rutin, syringin, kaempferol, kaempferol and quercetin in Gu-Hong injection were respectively 10.36 ~ 663.0 and 0.500 0 ~ 32.00 , 0.047 8 ~ 3.059,0.200 0 ~ 12.80,0.032 4 ~ 2.074,0.675 0 ~ 43.20,0.142 5 ~ 9.120μg · L -1, the average recoveries were 97.0% ~ 99.2% RSD <3.4% (n = 6). The mass concentration of seven components in three batches of samples was 28.5-32.4 g · L -1 for acetylglutamine, 1.02-1.23 g · L for hydroxysafflor yellow A ~ (-1), 14.3 ~ 17.6 mg · L -1 of rutin, 101 ~ 123 mg · L -1 of syringin, 12.1 ~ 14.9 μg · L -1 of beacon, 0.138 ~ 0.155 mg · L -1 of kaempferol and 73.4 ~ 95.6 μg · L -1 of quercetin. Conclusion: The method is simple, rapid, efficient, accurate and reliable and can be applied to the simultaneous determination of 7 effective metabolites of acetylglutamine, hydroxysafflor yellow A, rutin, syringin, kaempferol, kaempferol and quercetin Ingredients, provide a basis for the formulation of a more comprehensive quality control methods.