Wei Lili, Xue Xia, Liu Yanming, Sun Lizhen, Cheng Zhi, Su Shufang, Zhao Yin
Shandong Institute for Food and Drug Control, Jinan 250101, China.
Se Pu. 2019 Jul 8;37(7):735-741. doi: 10.3724/SP.J.1123.2019.01029.
An analytical method was developed for the determination of streptomycin and dihydrostreptomycin in honey using hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). The streptomycin and dihydrostreptomycin residues in the test samples were extracted with 20 g/L trichloroacetic acid aqueous solution (including 50 mmol/L phosphate, pH 6.8) and cleaned on an Oasis HLB solid phase extraction column. The products were separated on a SIELC Obelisc R column with gradient elution using 0.5% (v/v) formic acid aqueous solution and acetonitrile as mobile phases. Streptomycin and dihydrostreptomycin were detected by liquid chromatography-tandem mass spectrometry in the positive ion mode using the external standard method. Under the optimal conditions, streptomycin and dihydrostreptomycin showed good linearity (>0.99) in the range of 2.5-100 μg/L. The LOD and LOQ of the method was 2.0 μg/kg and 5.0 μg/kg, respectively. The spiked recoveries of the analytes from blank honey samples at the three levels of 5.0, 20.0 and 100.0 μg/kg were in the range of 86.9%-113.2% with the relative standard deviations less than 10%. With the advantages of convenience, rapidity, sensitivity and good repeatability, the method is suitable for the detection of streptomycin and dihydrostreptomycin in honey.
建立了一种采用亲水作用液相色谱 - 串联质谱法(HILIC - MS/MS)测定蜂蜜中链霉素和双氢链霉素的分析方法。测试样品中的链霉素和双氢链霉素残留用20 g/L三氯乙酸水溶液(含50 mmol/L磷酸盐,pH 6.8)提取,并在Oasis HLB固相萃取柱上进行净化。产物在SIELC Obelisc R柱上分离,以0.5%(v/v)甲酸水溶液和乙腈为流动相进行梯度洗脱。采用外标法,通过液相色谱 - 串联质谱在正离子模式下检测链霉素和双氢链霉素。在最佳条件下,链霉素和双氢链霉素在2.5 - 100 μg/L范围内呈现良好的线性关系(>0.99)。该方法的检出限和定量限分别为2.0 μg/kg和5.0 μg/kg。在5.0、20.0和100.0 μg/kg三个加标水平下,空白蜂蜜样品中分析物的加标回收率在86.9% - 113.2%范围内,相对标准偏差小于10%。该方法具有简便、快速、灵敏和重复性好等优点,适用于蜂蜜中链霉素和双氢链霉素的检测。