Determination of four ephedrine components in Banxialu granules by QuEChERS combined with UHPLC-MS/MS / 中国药房

ABSTRACT

OBJECTIVE To establish the met hod for the purific ation of test sample of Banxialu granules ，and to determine the contents of 4 ephedrine components such as ephedrine ，pseudoephedrine，norpseudoephedrine and methylephedrine. METHODS Three batches of Banxialu granules were extracted with methanol（containing 1％formic acid ）and pretreated with QuEChERS method of N-propyl ethylenediamine adsorbent （PSA）and octadecyl bonded silica gel adsorbent （C18）. Ultra high performance liquid chromatography tandem triple quadrupole mass spectrometry （UHPLC-MS/MS）was adopted. The separation was performed on an Agilent XDB-C 18 column with 5 mmol/L ammonium acetate solution （containing 0.1％ formic acid ）-acetonitrile as mobile phase（gradient elution ）at the flow rate of 0.40 mL/min. The column temperature was set at 30 ℃，and sample size was 2 μL. The electrospray ionization source was adopted ，and positive ion scanning was performed in multiple reaction monitoring mode. The ion pairs used for quantitative analysis were m/z 166.2→148.1（ephedrine，pseudoephedrine），m/z 152.2→134.1（norpseudoephedrine）， m/z 180.2→162.2（methylephedrine）. RESULTS The solution obtained by QuEChERS purification method was clear and nearly colorless. The linear ranges of ephedrine ， pseudoephedrine， norpseudoephedrine and methylephedrine were 1.38-206.82， 1.41-212.13，1.29-19.34，1.99-59.83 ng/mL（r＞0.99）. The limits of detection were 0.41，0.42，0.39 and 0.60 ng/mL. The limits of quantitation were 1.38 ，1.41 ，1.29 and 1.99 ng/mL，respectively. RSDs of precision ，stability（48 h）and repeatability tests were all lower than 2％. The average recoveries were 95.75％-100.87％（RSD＜2％，n＝9）. The contents of above 4 ephedrine components were 20.62-26.02，20.96-24.90，2.26-2.63，5.36-6.32 μg/g， respectively. CONCLUSIONS Established method is simple ，rapid，sensitive and suitable for simultaneous determination of 4 ephedrine components in Banxialu granules.