ABSTRACT
Objective To establish a UPLC-MS/MS method for determination of 10 anti-rheumatic constituents illegally added in Chinese traditional medicine and health products preparation.Methods The column was ACQUITY UPLC BEHC18 (50 mm× 2.1 mm,1.7 μm),The mobile phase was acetonitrile-Ammonium acetate solution (containing 0.1％ Acetic acid) with gradient elution at a flow rate of 0.3 mL/min.The ion source was electrospray ionization (ESI),Multiple-reaction monitoring (MRM) was performed to identify and quantify 10 anti-rheumatic constituents.Results 10 linear calibration curves were obtained with r ≥ 0.996 1.The recoveries were determinated at three concentration and ranged from 92.5％ to 101.8％.The precision of the method was shown by RSD (n =5) ranged from 0.9％ to 3.1％.The ranges of limit of detection were from 0.001 5 to 0.018 μg,and quantitation were from 0.004 5 to 0.55 μg.The illegally added chemicals were detected with 10 batches of 27 batches of samples.Conclusion The method were simple,sensitivity,accurate,and can be used to detect Anti-rheumatic constituents illegally added in Chinese traditional medicine and health products.
ABSTRACT
OBJECTIVE:To establish a rapid determination method for 9 kinds of glucocorticoid and 8 kinds of non-steroidal anti-inflammatory drugs illegally added into anti-rheumatic TCM patches. METHODS:UPLC-MS/MS method was adopted. The samples were separated on Acquity UPLC? BEN C18 column with methanol-water(90:10,V/V)as mobile phase at flow rate 0.4 mL/min. The column temperature was set at 30℃,and sample size was 1μL. The ionization mode was electrospray ion source(ESI):spray needle voltage of 5500 V,ion source spray GS1,GS2 pressure of 50,50 psi,ion source temperature of 500 ℃,scanning range of m/z 50-500. The multiple reaction monitoring(MRM)combined with information-dependent acquisition (IDA) and en-hanced product ion scanning(EPI)was used to rapid qualitative analysis. RESULTS:The detection limits for 17 kinds of chemical components were not more than 0.400 μg/mL. RSDs for precision,repeatability,stability tests were not more than 4.93%,7.69%, 9.57%,respectively. Diclofenac sodium was detected in the sample. CONCLUSIONS:The method is selective and sensitive. It is suitable for qualitative analysis of chemicals illegally added into anti-rheumatism TCM patches.
ABSTRACT
Objective: To develop a UPLC-MS/MS method for determination of eight antirheumatic cconstituents illegally added in Chinese patent medicine preparation. Methods: The analysis was performed by a UPLC-MS/MS system of Waters Acquity UPLC/ Quattro Premier, with BEH-C18 (100 mm × 2.1 mm, 1.7 μm) column. Multiple-reaction monitoring (MRM) was performed to identify and quantify hydrocortisone, dexamethasone, prednisone 21-acetate, 4-acetamidophenol, phenylbutazone, naproxen, piroxicam, and trimethoprim, which were extracted with methanol by ultrasonic method. Results: Eight linear calibration curves were obtained with r2 ≥ 0.998 9. The precision of the method was shown by RSD (n = 6) ranged from 1.2% to 3.5%. The recoveries were determinated at three concentration and ranged from 95.4% to 104.9%. The ranges of LLOQ were from 0.4 to 4.9 μg/mL and the RSDs (n = 9) of intra-day precision and inter-day precision were from 0.6% to 2.7% and from 0.9% to 2.9%. Conclusion: The method is specific, simple, and fast to detect eight antirheumatic constituents illegally added in Chinese patent medicine preparation.