固样(2.000 0 g)加水10.0 mL使其超声分散(液样取2.00 mL,加水8.0 mL),加甲醇稀释至50.0 mL.取上清液2.00 mL,用0.1 mol·L-1盐酸溶液稀释至10.0 mL.所得溶液经Cleanert PCX混合型阳离子固相萃取柱净化、氨水-甲醇(5+95)混合液洗脱.洗出液进行色谱分离,用ZORBAX SB-C18色谱柱作固定相,并以不同体积比的乙腈和0.01 mol·L-1乙酸铵溶液(pH 3.5)的混合液为流动相进行梯度淋洗.质谱分析中,采用电喷雾正离子源和多反应监测模式检测.13种壮阳类化合物的质量浓度在1.0～1 000 μg·L-1范围内呈线性,方法的检出限(3S/N)在3.0～40 μg·kg-1之间.加标回收率为80.1％～111％,相对标准偏差(n=6)小于8％.%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 HC1 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％.
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