Betteridge Keith, Cao Yu, Colegate Steven M
AgResearch Grasslands, Private Bag 11008, Palmerston North, New Zealand.
J Agric Food Chem. 2005 Mar 23;53(6):1894-902. doi: 10.1021/jf0480952.
A method for analyzing honey samples was developed that enabled the simultaneous detection and identification of pyrrolizidine alkaloids and their N-oxides. Honey samples were treated with methanol or dilute sulfuric acid and then centrifuged to remove insoluble material. Subsequent strong cation exchange, solid-phase extraction of the supernatant provided a fraction that was analyzed for the presence of pyrrolizidine alkaloids and their N-oxides using high-pressure liquid chromatography coupled to electrospray ionization mass spectrometry. The procedure was validated using extracts of Echium plantagineum and authenticated standards of pyrrolizidine alkaloids and their N-oxides from other plant sources. Of several variations of the solid-phase extraction method assessed in this study, the best combination for generic use involved the dilution of honey with 0.05 M sulfuric acid and the subsequent application of the centrifuged solution to solid-phase extraction columns at the rate of a maximum of 10 g of honey per solid-phase extraction column. The method was applied to the analysis of nine floral honeys, five of which were attributed by the apiarist to Echium vulgare. Seven of the honey samples were positive for pyrrolizidine alkaloids and N-oxides characteristic of E. vulgare.
开发了一种用于分析蜂蜜样本的方法，该方法能够同时检测和鉴定吡咯里西啶生物碱及其氮氧化物。蜂蜜样本用甲醇或稀硫酸处理，然后离心以去除不溶性物质。随后进行强阳离子交换，对上清液进行固相萃取，得到一个馏分，使用高压液相色谱-电喷雾电离质谱联用仪分析其中吡咯里西啶生物碱及其氮氧化物的存在情况。该方法使用蓝蓟提取物以及来自其他植物来源的吡咯里西啶生物碱及其氮氧化物的经鉴定标准品进行了验证。在本研究评估的几种固相萃取方法变体中，通用的最佳组合是用0.05 M硫酸稀释蜂蜜，随后将离心后的溶液以每个固相萃取柱最多10 g蜂蜜的速率应用于固相萃取柱。该方法应用于九种花蜜蜂蜜的分析，其中五种被养蜂人认为来自普通蓝蓟。七个蜂蜜样本对普通蓝蓟特有的吡咯里西啶生物碱和氮氧化物呈阳性。
