建立了一种固相萃取净化-超高效液相色谱-串联质谱检测蜂蜜中雷公藤次碱的分析方法。样品用水溶解后经固相萃取净化，采用 Hypersil GOLD C18柱（50 mm×2.1 mm，1.9μm）分离，以水和甲醇（含0．15％甲酸）为流动相，在流速0．25 mL／min下梯度洗脱，电喷雾离子源正离子多反应监测（ MRM）模式串联质谱进行测定。考察了试样溶解溶剂、色谱和质谱测定条件等。结果表明：雷公藤次碱在0.01~2μg／L范围内具有较好的线性关系，相关系数大于0.998。该方法定量限（ S／N＞10）为0.01μg／kg，在0.01、0.05和0.5μg／kg添加水平的回收率为76.1％~96.2％，相对标准偏差（ RSD，n=6）小于10％。该方法快速、灵敏、准确，适用于蜂蜜中雷公藤相关物质残留的定性、定量分析。
A method based on solid phase extraction and ultra performance liquid chromatogra-phy coupled with tandem mass spectrometry( SPE-UPLC-MS/MS)has been proposed for the determination of wilforine residue in honey. After the sample was dissolved with water,concen-trated and purified by an HLB solid phase extraction cartridge,the UPLC separation was per-formed on a Hypersil GOLD C18 column(50 mm×2. 1 mm,1. 9 μm)utilizing a gradient elution program of methanol( containing 0. 15% formic acid)and water as mobile phases at a flow rate of 0. 25 mL/min. The determination was carried out with electrospray ion source in the positive mode( ESI+)and multiple reaction monitoring( MRM)mode. The mass concentration of wilfo-rine in the range of 0. 01-2 μg/L was linearly correlated with the peak area,and the correlation coefficients was greater than 0. 998. The limit of quantification( S/N>10)for wilforine was 0. 01μg/kg. The recoveries were 76. 1% to 96. 2% in the spiked levels of 0. 01,0. 05 and 0. 5 μg/kg with the relative standard deviations( RSD,n=6)lower than 10%. The results indicate that the method is rapid,sensitive and accurate,and can be applied for the qualitative and quantitative analysis of wilforine in honey.
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