Determination of Residual Citrinin in Zhibituo Tablets by Solid Phase Extraction-UPLC-MS/MS / 中国药房

ABSTRACT

OBJECTIVE:To determine residual citrinin in Zhibituo tablet by solid phase extraction-UPLC-MS/MS. METH-ODSThe sample was processed preliminary by solid extraction. The determination was performed on Zorbax Eclipse Plus C18 col-umn with mobile phase consisting of water (0.1% formic acid)-acetonitrile (7030,V/V,gradient elution) at the follow rate of 0.30 mL/min. The column temperature was 40 ℃,and analysis time was 7 min,the sample size was 2 μL. Ionization mode was positive ion mode. The ion source temperature was 150 ℃,drying gas velocity was 15 L/min,sheath gas temperature was 350 ℃, sheath gas flow rate was 12 L/min,capillary voltage was 3500 V,atomization device pressure was 40 psi,atomization voltage was 0 V. The acquisition mode was MRM mode. RESULTS:The linear range of citrinin was 0.1-20 ng/mL(r=0.9994);the limits of quantitation and detection were 0.05 and 0.01 ng/mL. RSDs of precision,stability and repeatability tests were all lower than 2.0%;recoveries were 98.868%-103.160%(RSD=1.5%,n=6). CONCLUSIONS:The method is rapid,sensitive,accurate and suitable for the determination of residual citrinin in Zhibituo tablet.