Federal Office of Consumer Protection and Food Safety (BVL), National Reference Laboratories for Contaminants and Residues, Mauerstr. 39-42, 10117 Berlin, Germany.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2012;29(2):189-96. doi: 10.1080/19440049.2011.635347. Epub 2011 Dec 6.
A method was specifically developed for the determination and confirmation of streptomycin and dihydrostreptomycin in different types of honey. The method is simple, rapid, sensitive and was validated for streptomycin and dihydrostreptomycin in accordance with Commission Decision 2002/657/EC. After extraction with phosphate buffer and a pH change, clean-up was performed via SPE with polymeric phase. LC-MS/MS analysis was carried out using two different HILIC columns for the separation of the analytes and using a triple quadrupole mass spectrometer in positive ESI mode to measure the transitions of the substances in MRM mode. For the quantification of both substances, matrix calibration curves in a linear range of 5-80 g kg(-1) were used. The validation parameters established for streptomycin and dihydrostreptomycin, CCα (11.8 and 11.5 µg kg(-1), respectively), CCβ (18.9 and 19.9 µg kg(-1), respectively), recovery (97 and 101%, respectively) and the relative within-laboratory reproducibility RSD(wR) (16.4 and 20.8%, respectively) at the recommended concentration of 40 µg kg(-1), fulfil the requirements of Commission Decision 2002/657/EC.
一种专门用于检测和确认不同类型蜂蜜中链霉素和双氢链霉素的方法被开发出来。该方法简单、快速、灵敏，并且根据委员会 2002/657/EC 号决定对链霉素和双氢链霉素进行了验证。经过磷酸盐缓冲液提取和 pH 值改变后，通过聚合物相固相萃取进行净化。使用两种不同的亲水作用色谱柱进行分析物的分离，并用正电喷雾模式的三重四极杆质谱仪以 MRM 模式测量物质的跃迁，进行 LC-MS/MS 分析。对于这两种物质的定量，使用基质校准曲线在 5-80µgkg-1 的线性范围内进行。在推荐的 40µgkg-1 浓度下，建立的链霉素和双氢链霉素的验证参数，CCα（分别为 11.8 和 11.5µgkg-1）、CCβ（分别为 18.9 和 19.9µgkg-1）、回收率（分别为 97%和 101%）和相对实验室内部重现性 RSD（wR）（分别为 16.4%和 20.8%），满足委员会 2002/657/EC 号决定的要求。
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