磁性分散固相微萃取-超高效液相色谱-串联质谱法测定糖果中25种非法添加物

Determination of 25 kinds of illegal additives in candy by dispersive solid phase microextraction extraction-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  磁性分散固相微萃取  临床/违禁药物  超高效液相色谱-串联质谱法  非法添加物

英文关键词:dispersive solid phase microextraction extraction  clinical/illicit drugs  ultra performance liquid chromatography-tandem mass spectrometry  illegal additives

中文摘要:

      目的 建立磁性分散固相微萃取-超高效液相色谱-串联质谱法测定糖果中25种非法添加物。方法 样品采用50%甲醇水提取, 经磁性分散固相微萃取净化后由ACQUITY UPLC TSS T3色谱柱分离, 以甲酸铵水溶液-酸铵乙腈为流动相进行梯度洗脱, 经超高效液相色谱-串联质谱法测定, 外标法定量。结果 25种非法添加物在2.00~50.00 μg/L范围内线性关系良好, 相关系数(r2)>0.99, 回收率65.1%~99.3%, 相对标准偏差为1.1%~5.0%, 检出限0.05 mg/kg, 定量限0.10 mg/kg。应用该方法对105批次样品进行检测, 其中有1批次压片糖果中检出新利司他, 2批次糖果中检出双丙酚丁。结论 该方法采用磁性分散固相微萃取净化, 超高效液相色谱-串联质谱法检测, 准确性好, 灵敏度高, 能够满足糖果中25种非法添加物的检测需求。

英文摘要:

      Objective To establish a method for the determination of 25 kinds of illegal additives in candy by dispersive solid phase microextraction extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 50% methanol water, purified by dispersive solid phase microextraction extraction and separated by ACQUITY UPLC TSS T3 column. The samples were then eluted with ammonium formate aqueous solution and ammonium acetonitrile as mobile phase by gradient elution. The samples were determined by ultra performance liquid chromatography-tandem mass spectrometry and quantified by external standard method. Results The results showed that the 25 kinds of illegal additives had good linearity in the range of 2.00 to 50.00 μg/L with a correlation coefficient (r2) greater than 0.99, recoveries were between 65.1% and 99.3%, relative standard deviations were 1.1% to 5.0%, and limit of detection was 0.05 mg/kg and limit of quantification was 0.10 mg/kg. The method was applied to the detection of 105 batches of samples, in which one batch of compressed candy was found to contain xinlisita, and two batches of candy were found to contain dipropylphenidate. Conclusion The method is purified by dispersive solid phase microextraction extraction and detected by ultra performance liquid chromatography-tandem mass spectrometry. The method has good accuracy and high sensitivity, and can meet the detection requirements of 25 kinds of illegal additives in candy.