论文部分内容阅读
目的:建立五加生化胶囊UPLC-MS的指纹图谱,为科学客观地评价其质量提供可靠的方法。方法:色谱柱:ACQUITYUPLC BEH(2.1mm×50 mm,1.7μm);流动相:乙腈(A)-0.1%甲酸和10 mmol.L-1醋酸铵(B)梯度洗脱[5.0%A(0 min),5.0%A→50%A(0～10 min),50%A～80%A(10～16 min)];柱温:40℃;流速:0.4 mL.min-1;进样量:8μL;电喷雾接口,正离子模式,毛细管电压3.50 kV,锥孔电压35.00 V,离子源温度120℃,脱溶剂温度380℃,脱溶剂气N2:500 L.h-1,锥孔气N2:50 L.h-1。结果:11批五加生化胶囊UPLC-MS指纹图谱中共标定了37个共有色谱峰,通过与对照品的保留时间及质谱信息的比对,确定4号、8号、9号、10号和30号峰分别为紫丁香苷、阿魏酸、甘草苷、异嗪皮啶和藁本内酯。结论:所建立的五加生化胶囊UPLC-MS指纹图谱满足于方法学的要求,所得的指纹图谱特征性及专属性强,可用于五加生化胶囊质量的控制。
OBJECTIVE: To establish a fingerprint of UPLC-MS with five plus biochemical capsules to provide a reliable method for the scientific and objective evaluation of its quality. The mobile phase consisted of gradient elution of 5.0% A (0) with acetonitrile (A) -0.1% formic acid and 10 mmol·L -1 ammonium acetate (B) min), 5.0% A → 50% A (0-10 min), 50% A~80% A (10-16 min)]; column temperature 40 ° C .; flow rate 0.4 mL.min-1; : 8μL; electrospray interface, positive ion mode, capillary voltage 3.50 kV, cone voltage 35.00 V, ion source temperature 120 ℃, desolvation temperature 380 ℃, desolvation N2: 500 Lh-1, cone air N2: 50 Lh-1. Results: 37 common chromatographic peaks were identified in UPLC-MS fingerprints of 11 batches of five-plus biochemical capsules. Based on the comparison with the retention time and mass spectral data of the reference substance, the identification numbers of No.4, No.8, No.9, No.10 and No.3 Peaks were syringyl glycoside, ferulic acid, glycyrrhizin, isoindoline and ligustilide. Conclusion: UPLC-MS fingerprints of Wujia Biochemical Capsule are satisfied with the requirements of methodology. The obtained fingerprint is characterized by its specificity and specificity and can be used for the quality control of Wujia Biochemical Capsule.