Ma Xiao, Zuo Meng-Ting, Qi Xue-Jia, Wang Zi-Yuan, Liu Zhao-Ying
College of Veterinary Medicine, Hunan Agricultural University, Changsha 410128, China.
Hunan Engineering Technology Research Center of Veterinary Drugs, Hunan Agricultural University, Changsha 410128, China.
Foods. 2022 Sep 17;11(18):2891. doi: 10.3390/foods11182891.
Toxic Chinese medicine residues in honey pose a serious threat to consumer health. is one of the nine ancient poisons, making the whole plant virulent. The residue of alkaloid in honey causes poisoning from time to time. Therefore, it is very important to establish a method for the detection of alkaloids in honey. In this study, a method of solid phase extraction (SPE) with two-dimensional liquid chromatography (2D-LC) was developed for the first time for the simultaneous determination of alkaloids in honey, including gelsemine, koumine and humantenmine. First, the honey samples were purified by a PRS cation exchange column and extracted with 5% ammoniated methanol. Then, we verified the methodological indicators, which were in line with the Codex Guideline requirements. The verification results are as follows: matrix-matched calibrations indicated that the correlation coefficients were higher than 0.998. The recovery was in the range of 81%-94.2% with an intraday precision (RSD) of ≤5.0% and interday RSD of ≤3.8%. The limit of detection for the three alkaloids was 2 ng/g. The limits of quantification for gelsemine and koumine were 5 ng/g, and humantenmine was 20 ng/g. This method can be applied to the monitoring of alkaloids in honey.
蜂蜜中的有毒中药残留对消费者健康构成严重威胁。 是古代九大毒药之一，使整株植物都具有毒性。蜂蜜中生物碱的残留时常导致中毒。因此，建立一种检测蜂蜜中生物碱的方法非常重要。在本研究中，首次开发了一种二维液相色谱（2D-LC）结合固相萃取（SPE）的方法，用于同时测定蜂蜜中的生物碱，包括钩吻素甲、钩吻碱和胡蔓藤碱。首先，蜂蜜样品通过PRS阳离子交换柱纯化，并用5%氨化甲醇萃取。然后，我们验证了方法学指标，其符合食品法典指南要求。验证结果如下：基质匹配校准表明相关系数高于0.998。回收率在81%-94.2%范围内，日内精密度（RSD）≤5.0%，日间RSD≤3.8%。三种生物碱的检测限为2 ng/g。钩吻素甲和钩吻碱的定量限为5 ng/g，胡蔓藤碱为20 ng/g。该方法可应用于蜂蜜中生物碱的监测。
