高效液相色谱-串联质谱法检测宁南霉素在人参中的残留及消解规律

为明确宁南霉素在人参上的消解规律和最终残留水平,于2019年在吉林省白山市、抚松县、延吉市以及辽宁省桓仁县4地进行了宁南霉素在人参及其植株中的田间残留及消解动态试验.样品经体积分数为0.2％的甲酸水溶液提取,采用PLS+PXC固相萃取柱净化,XSelect?HSS T3色谱柱分离,高效液相色谱-串联质谱(HPLC-MS...

Residue and dissipation dynamics of ningnanmycin in ginseng by high performance liquid chromatography-tandem mass spectrometry

To investigate the dissipation and residues of ningnanmycin in ginseng, field trials of ningnanmycin residues in ginseng and its plants were conducted in Baishan City, Fusong County, Yanji City of Jilin Province, and Huanren County of Liaoning Province in 2019. The samples were extracted by 0.2% formic acid aqueous solution, cleaned up with PLS+PXC solid phase extraction column, separated by XSelect? HSS T3 column, and determined using HPLC-MS/MS. At 0.1, 0.2 and 1 mg/kg spiking levels, the average recoveries of ningnanmycin in fresh ginseng, ginseng plants were 90%-99%, 92%-94%, with the relative standard deviations (RSD) were 4.7%-5.6%, 4.0%-5.6%, respectively. At 0.2, 1 and 2 mg/kg spiking levels, the average recoveries of ningnanmycin in dried ginseng was 88%-95% with the RSD was 1.4%-10%. The limit of quantification (LOQ) of fresh ginseng and ginseng plants were both 0.1 mg/kg, and that of dried ginseng was 0.2 mg/kg. The results of the dissipation dynamic test in Baishan and Huanren showed that the half-lives of ningnanmycin on ginseng plants were 11.77 d and 0.76 d. The terminal residue results in 4 test places showed that the terminal residues of ningnanmycin on fresh ginseng, ginseng plants, and dried ginseng were