提出了固相萃取-超高效液相色谱-串联质谱法(SPE-UHPLC-MS/MS)测定丹参中30种禁用农药残留量的方法。样品粉末以0.5%(体积分数)乙酸溶液浸泡,乙腈振荡提取,提取液经ProElut SMC萃取柱净化。以Spursil C₁₈色谱柱(100 mm×2.1 mm,3.0 μm)为固定相,在梯度洗脱程序下分离30种禁用农药。以电喷雾离子源正离子模式扫描,多反应监测模式检测,采用基质匹配混合标准溶液绘制工作曲线,外标法定量。结果表明:30种禁用农药的质量浓度在一定范围内与对应的定量离子峰面积呈线性关系,测定下限(10S/N)为1~5 μg·L^-1;对空白样品进行3个浓度水平的加标回收试验,回收率为75.0%~120%,测定值的相对标准偏差(n=6)为1.2%~6.0%。方法用于市售丹参样品分析,一批样品中地虫硫磷和治螟磷的检出量分别为1.16 μg·kg^-1和0.37 μg·kg^-1,其余禁用农药均未检出。

A method for the determination of residues of 30 forbidden pesticides in Salvia miltiorrhiza by ultra-high performance liquid chromatography-tandem mass spectrometry with solid phase extraction (SPE-UHPLC-MS/MS) was proposed. Sample powder was soaked in 0.5% (volume fraction) acetic acid solution and then oscillated for extraction with acetonitrile, and the extract was purified by ProElut SMC extraction cartridge. Spursil C₁₈ column (100 mm×2.1 mm, 3.0 μm) was used as stationary phase, and the 30 forbidden pesticides were separated under gradient elution procedure. The analytes were scanned by electrospray ion source with positive ion mode, and detected by multi-reaction monitoring mode, and the matrix matching mixed standard solutions were used to draw working curves, with external standard method for quantitation. It was shown that linear relationships between the mass concentrations and corresponding quantitative ion peak areas of 30 forbidden pesticides were kept in definite ranges, with lower limits of determination (10S/N) in the range of 1-5 μg·L^-1. Test for recovery was made on the blank sample by standard addition method at 3 concentration levels, giving results in the range of 75.0%-120%, and RSDs (n=6) of the determined values ranged from 1.2% to 6.0%. This method was applied to analysis of the sold Salvia miltiorrhiza samples. The detection amounts of fonofos and sulfotep in one batch of sample were 1.16 μg·kg^-1 and 0.37 μg·kg^-1, respectively, and other forbidden pesticides were not detected.