摘要
建立了液相色谱-串联质谱（HPLC-MS/MS）法同时检测鳗鱼和蜂蜜中链霉素和双氢链霉素残留量的方法。样品用庚烷磺酸钠和磷酸盐缓冲液提取,经SUPELCO LC-C18固相萃取净化后,采用Thermo Aquasil-C18色谱柱（150 mm×4.6 mm,3μm）分离,以含0.3%乙酸的乙腈溶液和0.3%乙酸水溶液为流动相进行梯度洗脱,多反应监测模式测定,外标法定量。该方法在10～100μg/kg质量浓度范围内线性关系良好,定量下限均为10μg/kg。方法的回收率为89.6%～110.3%,相对标准偏差为2.3%～20.9%。该方法简便、实用、准确、快捷,能够满足蜂蜜和鳗鱼中链霉素和双氢链霉素残留量的检测需要。
A liquid chromatography coupled with tandem mass spectrometric（ LC-MS /MS） method was developed for the simultaneous determination of streptomycin and dihydrostreptomycin residues in eels and honey samples. The samples were extracted with sodium 1-heptanesulfonate and phosphate buffer,and cleaned up with a SUPELCO LC-C18solid phase extraction（ SPE） column. The extracts were separated on a Thermo Aquasil-C18column（ 150 mm × 4. 6 mm,3 μm） using acetonitrile containing 0. 3% acetic acid-0. 3% acetic acid as mobile phase by gradient elution. The detection of streptomycin and dihydrostreptomycin was carried out by MS /MS under multiple reaction monitoring（ MRM） mode. An external standard method was used for quantitative analysis. The method showed good linearities in the range of 10-100 μg /kg for streptomycin and dihydrostreptomycin,and the limits of quantitation（ LOQ） were 10 μg /kg. The spiked recoveries of streptomycin and dihydrostreptomycin ranged from 89. 6% to 110. 3% with relative standard deviations of 2. 3%-20. 9%. The method was simple,rapid and practical,and could meet the requirements for determination of streptomycin and dihydrostreptomycin residues in eel and honey samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第6期688-692,共5页
Journal of Instrumental Analysis
基金
上海技术标准专项资助(12DZ0503102)
关键词
液相色谱-串联质谱
蜂蜜
鳗鱼
链霉素
双氢链霉素
残留
liquid chromatography-tandem mass spectrometry（LC-MS /MS）
honey
eel
strep-tomycin
dihydrostreptomycin
residues
