HUANG Yue-yan;TU Jie-hong;XU Hong-xiang;FU Ying-hua
Chinese Traditional and Herbal Drugs,2016,Vol 47,No. 02
Objective: To estabilsh a rapid and accurate method for the determination of 17 anti-inflammatory and analgesic chemicals (paracetamol, aspirin, phenacetin, chlorpheniramine maleate, rofecoxib, piroxicam, lornoxicam, meloxicam, prednisone acetate, sulindac, naproxen, dexamethasone acetate, phenylbutazone, oxaprozin, celecoxib, diclofenac sodium, and indomethacin) which were illegally added into the Chinese patent medicines (CPM) and the health foods. Methods The UPLC-MS/MS method was adopted. The samples were extracted with methanol by ultrasonic processing and separated on a Waters Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with 0. 1% formic acid methanol (A) and 0.1% formic acid water (B) as the mobile phase by gradient elution (0–4 min, 40% A; 4–5 min, 40%–50% A; 5–6 min, 50%–60% A; 6–12 min, 60%–80% A; 12–13 min, 80% A; 13–14 min, 80%–40% A) at a flow rate of 0.2 mL/min, and the column temperature was 40 °C. A positive-ion (ESI+) source and a MRM mode were used to separately and quantitatively determinate the 17 anti-inflammation and analgesia chemicals. The obtained molecular ions, fragment ions, and retention time for MRM channels were used to identify the 17 chemicals by comparison with those of reference substances. The obtained peak areas were used to determinate the accurate content of chemicals in commonly used drugs in clinic. Results A good resolution of the 17 chemicals, including paracetamol, aspirin, phenacetin, chlorpheniramine maleate, rofecoxib, piroxicam, lornoxicam, meloxicam, prednisone acetate, sulindac, naproxen, dexamethasone acetate, phenylbutazone, oxaprozin, celecoxib, diclofenac sodium, and indomethacin were obtained under this UPLC and MS/MS condition. The limits of qualitation and quantitation were in the range of 0.3–5.0 and 0.9–15.0 ng/g. The standard addition recoveries were in the range of 90.5%–113.8%. The six components in samples (paracetamol, prednisone acetate, diclofenac sodium, indometacin, chlorpheniramine maleate, and naproxen) were detected. Conclusion The method is simple, accurate, and has high sensitivity, which can be used for the qualitative and quantitative determination of illegally added chemicals in CPM and health foods.
YU Fan;XU Xiao-gang;TANG Xin-hui;YANG Zhi-hui
Chinese Traditional and Herbal Drugs,2016,Vol 47,No. 02
Objective The process of preparing resveratrol orally disintegrating tablets was researched, the best prescription was determined and the quality of resveratrol orally disintegrating tablets about dissolution and micromeritics were evaluated. Methods The optimal prescription of direct powder compression method was determined by adopting Box-Benhnken center combination experiment design, with universal evaluation indexes, including disintegration time, mouthfeel, and hardness. The accumulative dissolution was tested by using dissolution test. The micromeritics about the angle of repose, loose density, tap density, and compressibility index were evaluated. Results The optimal prescription were 50 mg resveratrol (22.5%), 63.5 mg MCC (28.6%), 18.6 mg PVPP (8.4%), 10 mg L-HPC (4.5%), 78 mg (35.1%), and 2 mg magnesium stearate (0.9%). The disintegration time of resveratrol orally disintegrating tablets prepared with the optimized prescription was qualified. More than 90% resveratrol was dissoluted within 10 min. The micromeritics showed that the powder had good fluidity and filling property. Conclusion The process of preparation for orally disintegrating tablets by using direct compression method is feasible, it is easy to operate, and this method can meet the requirement in industry.
ZHANG Jin-hua;LIU Tao-shi;CHENG Jian-ming;CHEN Dong-dong;QIAN Hai-feng
Chinese Traditional and Herbal Drugs,2016,Vol 47,No. 02
Objective To explore the optimal separation and purification of extract in Sanao Sustained-release Tablets. Methods Taking the adsorption ratio and desorption ratio of ephedrine hydrochloride, pseudoephedrine hydrochloride, amygdalin, and glycyrrhizinate as evaluation indexes to optimize the purification process of Sanao Sustained-release Tablets by multi index comprehensive score. Results Macroporous resin HPD 300 had the best adsorption and desorption properties. In the course of adsorption, the optimum concentration of the sample liquid was 1.67 g crude drugs of per milliliter, the resin column size ratio was 1:7, the concentration of sample solution was 0.6 g/mL crude drug, and the sample flow rate was 4.0 BV/h. In the course of elution, 2 BV deionized water was used and the resin column chromatography was eluted with 5 BV of 70% EtOH by flow rate of 3 BV/h. Conclusion Macroporous resin HPD 300 is suitable to separate and purify the extract from Sanao Sustained-release Tablets.
