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.
| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |