Rapid determination of 17 anti-inflammatory and analgesic chemicals illegally added into Chinese patent medicine and health foods by UPLC-MS/MS / 中草药

ABSTRACT

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℃. 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 was 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.