超高效液相色谱-串联质谱法测定蔬菜水果中苦参碱残留量

Determination of matrine residues in vegetables and fruits by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  苦参碱  超高效液相色谱-串联质谱法  水果  蔬菜  基质效应

英文关键词:matrine  ultra performance liquid chromatography-tandem mass spectrometry  fruits  vegetables  matrix effect

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定蔬菜水果中苦参碱残留量的分析方法。方法 样品经乙腈提取, 乙二胺-N-丙基硅烷(primary secondary amine, PSA)净化。采用2 mmol乙酸铵(A)和甲醇(B)作为流动相进行梯度洗脱, 采用三重四极杆质谱对苦参碱进行检测定量。考察实验的重复性、苦参碱在各样品基质的基质效应及样品提取溶液的稳定性等指标。结果 本研究方法的条件下, 基质标准曲线方程为Y1=1180.6X1+63.317 (r2=0.9998), 试剂标准曲线方程为Y2=1831X2+404.28 (r2=0.9995)。检出限为2 μg/kg, 定量限可达到5 μg/kg。苦参碱在10种食品种类中在5、50和500 μg/kg 3个添加水平的回收率为69.88%~108.19%, 相对标准偏差(relative standard deviations, RSDs)均小于等于8.09% (n=6)。样品的重复性、稳定性较好, 均小于10%。结论 该方法快速、准确、灵敏, 适用于水果、蔬菜中苦参碱的大批量检测。

英文摘要:

      Objective To establish a method for the determination of matrine residues in vegetables and fruits by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by acetonitrile and purified by primary secondary amine (PSA). 2 mmol of ammonium acetate (A) and methanol (B) were used as mobile phase for gradient elution, and matrine was determined by triple quadrupole mass spectrometry. The experimental repeatability, the matrix effects of matrine in different food types, the stability of the extraction solution were also investigated. Results The standard curve in blank matrix was Y1=1180.6X1+63.317 (r2=0.9998), the standard curve in acetonitrile was Y2=1831X2+404.28 (r2=0.9995). The limit of detection of this method was 2 μg/kg and the limit of quantitation was 5 μg/kg. The recoveries of matrine at the levels of 5, 50 and 500 μg/kg in ten food types were 69.88%?108.19%, and relative standard deviations (RSDs) were less than 8.09% (n=6). The repeatability and stability of the samples were good, which were less than 10%. Conclusion The method is rapid, accurate, sensitive and suitable for mass determination of matrine in fruits and vegetables.