A simple but effective method was developed for the ultra-trace determination of two tropane alkaloid residues, hyoscyamine and scopolamine, in honey. Honey samples were dissolved in a concentrated aqueous solution of sodium acetate from which the alkaloids were subsequently extracted using acetonitrile. The resulting extract was analyzed using HILIC–ESI-MS/MS without any additional extract cleanup or enrichment steps. Enhanced sensitivity associated with the combination of HILIC and ESI-MS/MS techniques permitted the quantitation of the two tropane alkaloids at concentrations as low as 0.01 µg kg −1 . The use of isotopically labelled analogs permitted accuracies ranging from 86.9 to 106.1% for honey samples fortified at 0.02, 0.2 and 2 µg kg −1 with precisions ranging from 0.8 to 6.2%. The estimated method detection limits for hyoscyamine and scopolamine were 0.002 and 0.003 µg kg −1 , respectively. Twenty-three samples of honey were analyzed and only two samples were found to contain residues of the tropane alkaloids at concentrations above the limit of quantitation of 0.01 µg kg −1 . Hyoscyamine was detected at 0.012 µg kg −1 in two honey samples, one of which also contained 0.012 µg kg −1 of scopolamine.

中文翻译：

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HILIC–ESI-MS/MS 测定蜂蜜中的莨菪碱和东莨菪碱

开发了一种简单但有效的方法，用于超痕量测定蜂蜜中的莨菪烷和东莨菪碱两种托烷类生物碱残留量。将蜂蜜样品溶解在浓缩的乙酸钠水溶液中，随后使用乙腈从中提取生物碱。使用 HILIC-ESI-MS/MS 分析所得提取物，无需任何额外的提取物净化或富集步骤。与 HILIC 和 ESI-MS/MS 技术组合相关的增强灵敏度允许对浓度低至 0.01 µg kg -1 的两种托烷类生物碱进行定量。对于以 0.02、0.2 和 2 µg kg -1 进行强化的蜂蜜样品，同位素标记类似物的使用允许准确度范围为 86.9 至 106.1%，精度范围为 0.8 至 6.2%。莨菪碱和东莨菪碱的估计方法检测限分别为 0.002 和 0.003 µg kg -1 。对 23 个蜂蜜样品进行了分析，只有两个样品被发现含有浓度高于 0.01 µg kg -1 的定量限的托烷类生物碱残留物。在两个蜂蜜样品中检测到莨菪碱为 0.012 µg kg -1，其中一个还含有 0.012 µg kg -1 东莨菪碱。