液相色谱-三重四极杆质谱法测定花茶中5种吡咯里西啶类生物碱

Determination of 5 kinds of pyrrolizidine alkaloids in scented tea by liquid chromatography-triple quadrupole mass spectrometry

中文关键词:  液相色谱-三重四极杆质谱法  花茶  吡咯里西啶类生物碱

英文关键词:liquid chromatography-triple quadrupole mass spectrometry  scented tea  pyrrolizidine alkaloids

中文摘要:

      目的 建立液相色谱-三重四极杆质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS) 同时测定花茶中5种吡咯里西啶类生物碱含量的分析方法。方法 将花茶样品均质粉碎后, 经0.1%甲酸水溶液浸泡, 涡旋, 超声提取, 高速离心后取上清液过固相萃取柱, 洗脱液氮吹吹干后用流动相复溶, 经ZORBAX Eclipse PLUS C18色谱柱(2.1 mm×100 mm, 1.8 μm)分离, 以0.1%甲酸溶液和乙腈为流动相进行梯度洗脱, 流速为0.30 mL/min, 柱温为30 ℃, 多反应监测模式测定, 外标法定量。结果 该方法线性关系良好, 相关系数为0.997~0.998; 方法的检出限(S/N=3)为3~5 μg/kg、定量限(S/N=10)为10~15 μg/kg; 在15、30、150 μg/kg添加水平下的平均回收率为89.69%~102.12%, 相对标准偏差为0.3%~5.4%。结论 该方法样品前处理简单快速、萃取效果好、灵敏度和选择性高, 适用于常规检测。

英文摘要:

      Objective To establish a method for the determination of 5 kinds of pyrroliridine alkaloids in scented tea by liquid chromatography -tandem mass spectrometry (LC-MS/MS). Methods The sample was comminuted, and soaked in the aqueous solution of 0.1% formic acid, after vortex, ultrasonic extraction and high-speed centrifugation, and the supernatant was taken through the solid phase extraction column. After the eluting liquid nitrogen was blown and dried, the flow solution was re-dissolved. The samples were separated with a ZORBAX Eclipse PLUS C18 column (2.1 mm×100 mm, 1.8 μm) at the flow rate of 0.30 mL/min by gradient elution using 0.1% formic acid solution and acetonitrile as the mobile phase, and the column temperature was 30 ℃. The content of 5 kinds of pyrroliridine alkaloids was detected by multiple response monitoring model and quantitatively analyzed by external standard method. Results The linear relationship was good and the correlation coefficient was 0.997~0.998. The limit of detection of the method (S/N=3) was 3~5 μg/kg, the limit of quantitative (S/N=10) was 10~15 μg/kg, the average recovery rates at the addition levels of 15, 30, and 150 μg/kg were 89.69% to 102.12%, and the relative standard deviations were 0.3% to 5.4%. Conclusion This method is simple, rapid, effective, sensitive and selective, and suitable for conventional test.