SPE-UHPLC-MS/MS Determination of 13 Forbidden Male-genito-function-Strengthening Drugs in Traditional Chinese Medicines and Health-care Food

Solid sample (2.000 0 g) was dispersed ultrasonically in 10.0 mL of water, or 2.00 mL of liquid sample was mixed with 8.0 mL of water, and then diluted to 50.0 mL with CH₃OH. 2.00 mL of the supernatant was taken and diluted to 10.0 mL with 0.1 mol·L^-1 HCl solution, and then purified by passing through Cleanert PCX mixed cationic SPE column, which was then eluted with a mixture of aq. ammonia and methanol (5+95). The eluate was separated on ZORBAX SB-C₁₈ column using mixtures of 0.01 mol·L^-1 NH₄OAc solution (pH 3.5) and acetonitrile in various ratios as mobile phase in gradient elution. ESI⁺ and MRM were adopted in MS. Linear relationships between values of peak areas and mass concentrations of the 13 forbidden drugs were obtained in the same range of 1.0-1 000 μg·L^-1, with values of detection limits (3S/N) in the range of 3.0-40 μg·kg^-1. Tests for recovery were made by standard addition method, giving values of recovery in the range of 80.1%-111%, with values of RSDs (n=6) less than 8%.