LC-MS/MS法同时测定不同产地半枝莲中野黄芩苷和芹菜素含量

LC-MS/MS simultaneous determination of scutellarin and apigenin of Herba Scutellariae Barbatae produced in different districts

目的:采用液相色谱-二级质谱联用法(LC-MS/MS)对不同产地半枝莲药材中的野黄芩苷和芹菜素进行含量测定。方法:采用Discovery C18柱(250mm×4.6mm,5μm),流动相为乙腈-0.1%醋酸,梯度洗脱,流速1mL·min-1,测定波长335nm,采用电喷雾负模式电离(ESI-),选定的母离子和子离子分别为野黄芩苷m/z461/285,芹菜素m/z269/117。结果:野黄芩苷浓度在2.6～72.7mg·L-1,芹菜素浓度在2.3～63.8mg·L-1范围内线性关系良好;所测12个产地半枝莲中,野黄芩苷和芹菜素的含量范围分别为0.03%～0.39%和0.02%～0.30%;平均回收率(n=5)分别为99.1%和97.3%,RSD分别为1.4%和0.7%。结论:本方法简单准确,适合于半枝莲中野黄芩苷和芹菜素的含量测定。

Objective ：To detect and quantificate scutellarin and apigenin in Herba Scutellariae Barbatae of differ- ent districts by LC -MS/MS. Methods：Determination of LC system consisted of a Discovery C t8 column（250 mm × 4. 6 mm,5μm） with acetonitrile and water（O. 1% acetic acid） in linear gradient condition. The flow rate was 1 mL · min-1 mm and the wavelength of detection was 335 nm. The mass spectrometer was operated under the negative ion mode with the ESI source. The transition of m/z 461/285 and m/z 269/117 was used to qualify scutellarin and api- genin, respectively. Results：The linear ranges of calibration curve of scutellarin and apigenin were 2. 6 -72. 7 mg · L-1and 2. 3 -63.8 mg · L-1, respectively. By using the established LC -MS/MS methods, 12 samples of Herba Scutellariae Barbatae in different districts were analyzed. The results showed that the contents of scutellarin and api- genin were 0. 03% -0. 39% and 0. 02% -0. 30% , respectively. The average recoveries（ n = 5 ） of scutellarin and apigenin were 99. 1% and 97.3 %, and the RSDs were 1.4% and 0. 7%, respectively. Conclusion：The proposed method is simple and the result is accurate. It can be used for determination of scutellarin and apigenin in Herba Scutellariae Barbatae.