Simultaneous determination of four effective components in Guilin Watermelon Frost by HPLC-MS / 中成药

ABSTRACT

AIM: To establish an HPLC-MS method for simultaneously determining four effective components in Guilin Watermelon Frost(Mirabilitum Praeparatum,Rhizoma Coptidis,Radix Scutellariae,etc.). METHODS: The sample was extracted with methanol containing 20% chloroform under ultrasonication.The HPLC separation was performed on Zorbax SB C_(18)(3.0 mm?250 mm,5 ?m) column using water including 0.5% formic acid(A)-methanol(B) as mobile phase,with the gradient elution(0-2 min,60%B;2-5 min,60%→90%B;5 min to the end,90%B), at a flow rate of 0.40 mL/min.The compounds were analyzed by ESI-MS under ion monitoring mode(0-3 min,m/z 249;3-6 min,m/z 336;6-10 min,m/z 447;10-16 min,m/z 263). RESULTS: The linear ranges were 0.020-10.0 ?g/mL,0.010-40.0 ?g/mL,0.036-50.0 ?g/mL and 0.040-4.00 ?g/mL for matrine,berberine,baicalin and indirubin,with detection limits of 0.005,0.001,0.006 and 0.010 ?g/mL,respectively.The average recoveries ranged from 96% to 101% with all relative standard deviations less than 3%.CONCLUSION: (The method is rapid,accurate and suitable for the quality control of the four effective) components in Guilin Watermelon Frost.