ABSTRACT
Objective To establish HPLC method for simultaneous determination of five active ingredients of cucurbitacin B, cucurbitacin E, praeruptorin A, praeruptorin B, and praeruptorin E in Infantile Qingfei Pills (IQP), and study the contents changes of the five effective components in IQP before and after 60Co-γ ray irradiation. Methods The Agilent-C18 column (250 mm × 4.6 mm, 5 μm) was adopted and the detection wavelength was 230 nm and 321 nm with the flow rate of 1.0 mL/min. The mobile phase consisted of A (methanol: acetonitrile) and B (0.5% glacial acetic acid solution) for gradient elution, and column temperature was 25 ℃. Irradiation does of 2, 4, 6, 8 kGy were selected to irradiate IQP respectively. The contents of five active components in IQP were compared before and after irradiation, and the significant condition was observed by t-test. Results The linear range of cucurbitacin B, cucurbitacin E, praeruptorin A, praeruptorin B, and praeruptorin E were 0.049—1.247, 0.079—1.973, 0.056—1.406, 0.028—0.705, and 0.028—0.693 μg, The average recovery were 101.2%, 99.7%, 99.9%, 98.9%, and 100.5%, and RSD were 0.6%, 0.5%, 1.2%, 1.1%, and 1.2%, respectively. After irradiation of 2, 4, 6, and 8 kGy, the effective components contents of cucurbitacin B, cucurbitacin E, praeruptorin A, praeruptorin B, and praeruptorin E were changed. After t-test in groups, the content change of cucurbitacin B was significantly after irradiation over 6 kGy (P < 0.05). Conclusion The established method has a high recovery rate, good repeatability, which is simple and practical and can be used for quality control of IQP. The changes of each component are not significant with the radiation no more than 6 kGy, which can provide a reference for the sterilization of IQP.
ABSTRACT
Objective To establish a method for content determination of praeruptorin A and praeruptorin B in Tongxuan Lifei Pills. Methods UPLC method was adopted. ACE UItra Core Super C18 (75 mm × 2.1 mm, 2.5 μm) was used with methanol-water as the mobile phase, by gradient elute. The flow rate was 0.3 mL/min; The detection wavelength was set at 321 nm; The column temperature was 40 ℃. Results Praeruptorin A and praeruptorin B showed the good linear relationship in the range of 20.48–204.8 ng (r=0.999 7) and 5.158–51.58 ng (r=1.000 0), respectively. The average recoveries were 98.2％ and 100.3％, respectively. Conclusion The method is simple, fast, accurate and reproducible, which can be used to determine the contents of praeruptorin A and praeruptorin B in Tongxuan Lifei Pills.
ABSTRACT
Objective: To establish a UPLC/Q-TOF MS method for analyszing the chemical constituents of total coumarins extract from Peucedani Radix (the rhizome of Peucedanum praeruptorum) and to study its preliminary pharmacodynamics. Methods: The chromatographic column was Acquity UPLC BEH C18, the mobile phase was composed of 0.1% formic acid (A) and acetonitrile (B) with gradient elution; The detection wavelength was set at 321 nm; The ionization mode was ESI+; And the mass scan range was m/z 100-1 000. Using the rat model of type 2 diabetes mellitus (T2DM) induced by streptozocin (STZ), the effect of total coumarins on reducing blood-lipid and blood-sugar was investigated in the experiment. Results: Qianhucoumarin D, peucedanocoumarin II, praeruptorin A, peucedanocoumarin I, praeruptorin B, and praeuptorin E in Peucedani Radix coumarin could be well separated and identified in one run. The preliminary pharmacodynamic results show that the total coumarins had an effect of reducing the level of fasting blood glucose, cholesterol, triglycerides, LDL, and liver index (P < 0.05); On the other hand, it could improve the level of HDL (P < 0.05). The above results prompt that coumarin extract of Peucedani Radix could improve the carbohydrate and lipid metabolism of T2DM, then play a role in the treatment of T2DM. Conclusion: A UPLC/Q-TOF MS method has been established to separate and identify the total coumarin extract of Peucedani Radix, the preliminary pharmacodynamic study shows that the total coumarin extract of Peucedani Radix had the function of reducing blood sugar and blood lipid significantly.
ABSTRACT
@#(±)-Praeruptorin A(PA)was used as the standard reference substance to establish a new method of substitute for reference substance. The contents of both(±)-praeruptorin B(PB)and(+)-praeruptorin E(PE)were calculated by the method. The major content of coumarins in different processing materials could be gained by determining the content of(±)-praeruptorin A, which could provide scientific evidence for the research on pharmacology discrepancy and quality standards. The method was carried out on a Welch Materials Ultimate XB-C18 column(4. 6 mm×250 mm, 5 μm), with a gradient mobile phase of methanol and water at the flow rate of 1. 0 mL/min. The column temperature was 30 °C and detection wavelength was set at 322 nm. According to this method, the relative correlation factors(f)of(±)-praeruptorin B and(+)-praeruptorin E were determined as 0. 787 2 and 0. 969 0, respectively. After determine the contents of 15 batches of materials from different sources, no significant differences between substitute method and external standard method were observed. It was a feasible and credible method to determine the content of major coumarins in Peucedani Radix with different processing materials. The results showed lower contents of coumarins in processing materials than in raw materials.