ABSTRACT
Objective To comparative analyze the contents of 20 active ingredients in two dosage forms of Zhizhu Pills (ZP) and Zhizhu Granules (ZG). Methods Three batches of raw materials were used for the preparation of ZP and ZG according to the preparation process of China Pharmacopoeia (2015 Editon). Twenty active ingredients in the two dosage forms were detected simultaneously using high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-QqQ-MS). The separation was performed on a Poroshell 120 SB-C18 (100 mm × 4.6 mm, 2.7 μm) column with a flow rate of 0.5 mL/min. Mobile phase consisted of 0.1% formic acid in water (A)-0.1% formic acid in acetonitrile (B). The column temperature was set at 30 ℃. The gradient elution conditions: 0-7 min, 23% B; 7-17 min, 23%-80% B; 17-20 min, 80%-100% B, 20-30 min, 100% B; flow rate was 0.5 mL/min. Results The contents of 20 active ingredients in the pills were 1.48-13.37 times that of the granules, the total difference of them perday were 493.02-615.08 mg. Conclusion There were significant differences in the content of active components in the two dosage forms of ZP and ZG, especially those components with poor solubility in water and thermal instability.
ABSTRACT
OBJECTIVE: To establish a UHPLC-MS/MS method for simultaneous determination of tangertin, hesperetin, 5-demethylnobiletin, nobiletin, vitexin, and narirutin in Rukuaixiao granules. METHODS: The analysis method was performed on a Waters ACQUITY UPLC® BEH C18 eolumn (2.1 mm×50 mm, 1.7 μm) with gradient elution of acetonitrile (containing 0.1% formic acid)-0.1% formic acid at a flow rate of 0.6 mL·min-1, and the column temperature was set at 50℃. Electrospray ionization (ESI) source with positive mode and the detector with multiple reaction monitoring (MRM) mode were adopted to determine the analytes by mass spectormeter. RESULTS: Satisfactory linearities were obtained for the six constituents in the investigated ranges (r>0.9958): The lower limit of quantitation (LOQ) was 0.80, 1.10, 1.30, 0.66, 2.00, 7.10 and 0.70 ng·mL-1, respectively. All the recoveries of samples were between 95.78%-101.35% with RSDs less than 2.1%. CONCLUSION: The method is simple, rapid, sensitive, and highly reproducible. It can be applied to the quality control of Rukuaixiao granules.