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UPLC-MS/MS同时测定金牡感冒片中15个成分 被引量:2

Simultaneous determination of fifteen components in Jinmu Ganmao tablets by UPLC-MS/MS
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摘要 目的:建立超高效液相色谱串联质谱法(UPLC-MS/MS法)同时测定金牡感冒片中15个化学成分(新绿原酸、原儿茶酸、对羟基苯甲酸、绿原酸、隐绿原酸、獐牙菜苷、夏佛塔苷、穗花牡荆苷、异夏佛塔苷、牡荆素鼠李糖苷、牡荆苷、木犀草苷、异绿原酸B、异绿原酸A、异绿原酸C)的含量。方法:采用UPLC-MS/MS法,正负离子切换的多反应监测(MRM)模式进行含量测定。色谱条件:使用CORTECS UPLC C_(18)色谱柱(100 mm×2.1 mm,1.6μm),流动相为0.1%甲酸水-乙腈,梯度洗脱,流速为0.25 m L·min^-1。结果:15个成分在各自考察的浓度范围内线性关系良好,相关系数(r)均大于0.994 0;加样回收率在96.8%~104.5%,RSD为3.8%~4.6%;12批样品中新绿原酸、原儿茶酸、对羟基苯甲酸、绿原酸、隐绿原酸、獐牙菜苷、夏佛塔苷、穗花牡荆苷、异夏佛塔苷、牡荆素鼠李糖苷、牡荆苷、木犀草苷、异绿原酸A、B、C的含量分别为0.300~0.630、0.013~0.031、0.053~0.133、2.319~4.290、0.442~0.792、0.345~0.715、0.476~0.945、0.164~0.283、0.068~0.162、0.004~0.006、0.006~0.013、0.064~0.100、0.974~1.682、0.423~0.690、0.799~1.636 mg·g^-1。结论:本研究所建立的UPLC-MS/MS定量分析方法可作为金牡感冒片中15个成分同时测定的方法。 Objective:To establish an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of 15 components (neochlorogenic acid, protocatechuic acid, 4-hydroxybenzoic acid, chlorogenic acid, cryptochlorogenin acid, sweroside, schaftoside,agnuside, isoschaftoside, vitexin-2-O-rhamnoside, vitexin, luteolin, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C ) in Jinmu Ganmao tablets. Methods: The separation was performed on a CORTECS UPLC Cls column ( 100 mm × 2. 1 mm, 1.6 μm ). Acetonitrile and water( containing 0. 1% formic acid )were adopted as the mobile phase by gradient elution at a flow rate of 0. 25 mL· min^-1. MS detection was performed with multiple reaction monitoring mode. Results: The developed method showed good linearity ( r 〉 0. 994 0 ) for all the analytes within the test ranges. The overall average recovery rates were in the range of 96. 8%-104. 5% with RSD of 3.8%-4.6%. The contents of neochlorogenic acid, protocatechuic acid, 4-hydroxybenzoic acid, chlorogenic acid, cryptochlorogenin acid, sweroside, schaftoside, agnuside, isoschaftoside, vitexin-2-O-rhamnoside, vitexin, luteolin, isochlorogenic acid A, B and C in twelve samples were 0. 300-0. 630 mg·g^-1 O. 013-0. 031 mg·g^-1, 0. 053-0. 133 mg·g^-1, 2. 319-4. 290 mg·g^-1, 0. 442-0. 792 mg·g^-1, 0. 345-0. 715 mg·g^-1, 0. 476-0. 945 mg·g^-1, 0. 164-0. 283 mg·g^-1, 0. 068-0. 162 mg·g^-1, 0. 004-0. 006 mg·g^-1, 0. 006-0. 013 mg·g^-1, 0. 064- 0. 100 mg·g^-1, 0. 974-1.682 mg·g^-1, 0. 423--0. 690 mg·g^-1 and 0. 799-1. 636 mg·g^-1, respectively. Conclusion: The UPLC-MS/MS method could be used for the quality control of Jinmu Ganmao tablets.
作者 黄秋妹 许舒瑜 邰艳妮 沈少君 郭慧婷 黄鸣清 HUANG Qiu-mei1, XU Shu-yu2, TAI Yan-ni2, SHEN Shao-jun2, GUO Hui-ting2, HUANG Ming-qing2 ( 1. Guangdong Food and Drug Vocational College, Guangzhou 510520, China; 2. School of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350122, China )
出处 《药物分析杂志》 CSCD 北大核心 2017年第8期1453-1460,共8页 Chinese Journal of Pharmaceutical Analysis
基金 福建省教育厅高校新世纪优秀人才支持计划(闽教科(2015)54号) 福建省大学生创新创业训练项目(201610393010)
关键词 金牡感冒片 新绿原酸 原儿茶酸 对羟基苯甲酸 绿原酸 隐绿原酸 獐牙菜苷 夏佛塔苷 穗花牡荆苷 异夏佛塔苷 牡荆素鼠李糖苷 牡荆苷 木犀草苷 异绿原酸 黄酮 酚酸 环烯醚萜苷 含量测定 超高效液相色谱串联质谱 Jinmu Ganmao tablets neochlorogenic acid protocatechuic acid 4-hydroxybenzoic acid chlorogenic acid eryptochlorogenin acid sweroside schaftoside agnuside isoschaftoside vitexin-2-O-rhamnoside vitexin luteolin isochlorogenic acid flavonoids phenolic acids iridoid glycosides quantitative analysis UPLC-MS/MS
作者简介 第一作者Tel:(020)28854884;E-mail:huang1596@163.com 通信作者Tel:(0591)22861135;E-mail:hmq1115@126.com
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