固相萃取净化-超高效液相色谱-串联质谱法测定蜂蜜中雷公藤次碱

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, 1.9 μm)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0.01~2 μg/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0.01 μg/kg,在0.01、0.05和0.5 μg/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.

Determination of wilforine in honey using solid phase extraction purification and ultra performance liquid chromatography-tandem mass spectrometry

A method based on solid phase extraction and ultra performance liquid chromatography 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, concentrated and purified by an HLB solid phase extraction cartridge, the UPLC separation was performed 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 wilforine 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 0.01 μg/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.