UPLC-MS/MS同时测定金牡感冒片中15个成分

Simultaneous determination of fifteen components in Jinmu Ganmao tablets by UPLC-MS/MS

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.