UPLC-MS/MS同时测定青钱柳中6种黄酮类成分

陈张金; 余华丽<sup>*</sup>; 毛菊华; 范蕾; 王伟影

引用本文:	陈张金,余华丽,毛菊华,范蕾,王伟影.UPLC-MS/MS同时测定青钱柳中6种黄酮类成分[J].中国现代应用药学,2021,38(2):201-206.
	CHEN Zhangjin,YU Huali,MAO Juhua,FAN Lei,WANG Weiying.Simultaneous Determination of Six Flavonoids in Cyclocarya Paliurus by UPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2021,38(2):201-206.

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UPLC-MS/MS同时测定青钱柳中6种黄酮类成分
陈张金^1,2, 余华丽², 毛菊华², 范蕾², 王伟影^1,2
1.浙江中医药大学, 杭州 310053;2.丽水市质量检验检测研究院, 浙江丽水 323000

摘要:

目的建立UPLC-MS/MS同时测定青钱柳中芦丁、金丝桃苷、槲皮素-3-O-葡萄糖醛酸苷、异槲皮苷、槲皮苷、槲皮素6种黄酮类成分的分析方法。方法超高效液相法采用色谱柱为Agilent ZORBAX RRHD SB-C₁₈（2.1 mm×100 mm，1.8 μm），流动相为乙腈-0.1%甲酸水溶液，梯度洗脱，流速为0.3 mL·min^-1，柱温40℃，进样量为1 μL；质谱法采用三重四级杆质谱，电喷雾离子源、负离子模式（ESI^-），通过多重反应监测同时对青钱柳中6种黄酮类成分进行定量分析。结果测定青钱柳中6种黄酮类成分芦丁、金丝桃苷、槲皮素-3-O-葡萄糖醛酸苷、异槲皮苷、槲皮苷、槲皮素的线性范围分别为0.002~0.24 μg·mL^-1（R²=0.999 4），0.049~4.91 μg·mL^-1（R²=0.999 5），0.504~50.37 μg·mL^-1（R²=0.999 4），0.051~5.12 μg·mL^-1（R²=0.999 4），0.005~0.52 μg·mL^-1（R²=0.999 8），0.052~5.17 μg·mL^-1（R²=0.999 9），平均回收率分别为96.1%，98.4%，98.5%，97.3%，96.7%，96.5%，RSD分别为1.78%，1.22%，1.91%，1.08%，1.21%，1.29%； 16批青钱柳样品中6种黄酮的含量分别为0.019 8~0.253 7 ，0.923 5~15.568 0 ，12.987 8~130.510 9 ，0.122 9~12.101 1 ，0.007 4~0.573 9 ，0.387 7~12.456 7 mg·g^-1，其中槲皮素-3-O-葡萄糖醛酸苷的含量最高，约占总量的78%。结论所建立的分析方法简单、快速、灵敏度高、专属性好，可应用于青钱柳中黄酮类成分的含量测定及质量控制。

关键词: 青钱柳异槲皮苷槲皮素-3-O-葡萄糖醛酸苷黄酮液质联用法

DOI：10.13748/j.cnki.issn1007-7693.2021.02.013

分类号:R917

基金项目:丽水市科技计划项目（2017GYX47）

Simultaneous Determination of Six Flavonoids in Cyclocarya Paliurus by UPLC-MS/MS

CHEN Zhangjin^1,2, YU Huali², MAO Juhua², FAN Lei², WANG Weiying^1,2

1.Zhejiang Chinese Medical University, Hangzhou 310053, China;2.Lishui Institute for Quality Inspection and Testing, Lishui 323000, China

Abstract:

OBJECTIVE To develop an UPLC-MS/MS method for simultaneously determination of six flavonoids(rutin, hyperoside, quercetin-3-O-glucuronide, isoquercitrin, quercitrin, quercetin) in Cyclocarya paliurus. METHODS The UPLC method was performed on an Agilent ZORBAX RRHD SB-C₁₈ column(2.1 mm×100 mm, 1.8 μm) with a gradient elution of acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL·min^-1, the column temperature was 40℃, and the injection volume was 1 μL; mass spectrometry used the triple quadrupole mass spectrometry, electrospray ionization source, negative mode(ESI^-) and the multiple reaction monitoring mode was employed for the quantitative analysis of six flavonoids. RESULTS The linear ranges of rutin, hyperoside, quercetin-3-O-glucuronide, isoquercitrin, quercitrin and quercetin were 0.002-0.24 μg·mL^-1 (R²=0.999 4), 0.049-4.91 μg·mL^-1(R²=0.999 5), 0.504-50.37 μg·mL^-1(R²=0.999 4), 0.051-5.12 μg·mL^-1(R²=0.999 4), 0.005-0.52 μg·mL^-1(R²=0.999 8), 0.052-5.17 μg·mL^-1(R²=0.999 9); the average recoveries were 96.1%, 98.4%, 98.5%, 97.3%, 96.7%, 96.5%, respectively. The RSDs were 1.78%, 1.22%, 1.91%, 1.08%, 1.21%, 1.29%, respectively. The content of six flavonoids in 16 batches were 0.019 8-0.253 7, 0.923 5^-15.568 0, 12.987 8^-130.510 9, 0.122 9^-12.101 1, 0.007 4-0.573 9, 0.387 7^-12.456 7 mg·g^-1, respectively, and the content of quercetin-3-O-glucuronide was the highest, which accounted for about 78% of the total amount. CONCLUSION The developed method is simple, rapid, sensitive and specific, which can be used for the determination of flavonoids and the quality control of Cyclocarya paliurus.

Key words: Cyclocarya paliurus isoquercitrin quercetin-3-O-glucuronide flavonoids UPLC-MS/MS