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亲水作用液相色谱-串联质谱法测定蜂蜜中链霉素和双氢链霉素残留量

[Determination of streptomycin and dihydrostreptomycin residues in honey by hydrophilic interaction liquid chromatography-tandem mass spectrometry].

作者信息

Wei Lili, Xue Xia, Liu Yanming, Sun Lizhen, Cheng Zhi, Su Shufang, Zhao Yin

机构信息

Shandong Institute for Food and Drug Control, Jinan 250101, China.

出版信息

Se Pu. 2019 Jul 8;37(7):735-741. doi: 10.3724/SP.J.1123.2019.01029.

Abstract

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.

摘要

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。

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