弱阳离子交换固相萃取-超高效液相色谱-串联质谱法测定牛奶中13种氨基糖苷类药物残留  

Determination of 13 Aminoglycoside Residues in Milk by Weak Cation Exchange Solid Phase Extraction Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：何金麟 沈鹭英 孙婷 傅建炜[2] 严丽娟 徐敦明 HE Jinlin;SHEN Luying;SUN Ting;FU Jianwei;YAN Lijuan;XU Dunming(Technical Center of Xiamen Customs,Xiamen 361026,China;Fujian Key Laboratory of Agro-products Quality and Safety,Fujian Academy of Agricultural Sciences,Fuzhou 350003,China)

机构地区：[1]厦门海关技术中心,福建厦门361026 [2]福建省农业科学院,福建省农产品质量安全重点实验室,福建福州350003

出　　处：《食品科学》2025年第3期238-245,共8页Food Science

基　　金：福建省农产品质量安全重点实验室开放课题项目(KFKT2020-4);“十四五”国家重点研发计划重点专项(2023YFF1104900)。

摘　　要：本研究建立弱阳离子交换固相萃取-超高效液相色谱-串联质谱测定牛奶中13种氨基糖苷类药物(安普霉素、阿米卡星、巴龙霉素、潮霉素B、核糖霉素、卡那霉素、链霉素、庆大霉素C1、双氢链霉素、妥布霉素、壮观霉素、新霉素和小诺霉素)的检测方法。牛奶样品经乙酸铵缓冲溶液和乙腈提取,弱阳离子交换固相萃取柱净化,SILICA SG80液相色谱柱分离。采用0.1%甲酸溶液和乙腈作为流动相进行梯度洗脱,在电喷雾电离源、正离子模式下进行超高效液相色谱-串联质谱检测,采用基质匹配标准外标法定量。在5.0~500.0 ng/mL范围内,13种氨基糖苷类药物呈现良好的线性关系(R^(2)≥0.998 3)。潮霉素B、核糖霉素、链霉素、妥布霉素和双氢链霉素的检出限均为3μg/kg,定量限均为10μg/kg;安普霉素、阿米卡星、巴龙霉素、卡那霉素、庆大霉素C_(1)、小诺霉素、新霉素和壮观霉素的检出限均为15μg/kg,定量限均为50μg/kg。在1、2倍和5倍的定量限加标水平下,回收率为73.8%~107.4%,相对标准偏差为1.0%~9.8%。该方法灵敏度高、操作简单、稳定性好,可用于检测牛奶中13种氨基糖苷类药物。In this study,a method based on weak cation exchange(WCX)solid phase extraction(SPE)coupled with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the simultaneous determination of 13 aminoglycoside(apramycin,amikacin,paromomycin,hygromycin B,ribostamycin,kanamycin,streptomycin,gentamicin C1,dihydrostreptomycin,tobramycin,spectinomycin,neomycin and micronomicin)residues in milk.Samples were extracted using a mixture of ammonium acetate buffer solution and acetonitrile,and purified using a WCX SPE column.Chromatographic separation was achieved using a SILICA SG80 column with gradient elution using a mobile phase made up of 0.1%formic acid aqueous solution and acetonitrile.Detection was accomplished using an electrospray ionization source(EIS)in the positive ion mode,and quantification was carried out using a matrix-matched external standard method.Excellent linear relationships were observed for the 13 aminoglycosides in the concentration range of 5.0-500.0 ng/mL(R^(2)≥0.9983).The limit of detection(LOD)for hygromycin B,ribostamycin,streptomycin,tobramycin,and dihydrostreptomycin were 3μg/kg,and the limit of quantification(LOQ)were all 10μg/kg for these aminoglycosides.For apramycin, amikacin, paromomycin, kanamycin, gentamicin C_(1), micronomicin, neomycin and spectinomycin, the LODs and LOQs were 15 and 50 μg/kg, respectively. The recovery rates of milk spiked at 1 ×, 2 × and 5 × LOQ levels were 73.8%-107.4%, with relative standard deviation (RSD) of 1.0%-9.8%. This developed method is sensitive, simple, stable, and suitable for the determination of these 13 aminoglycoside residues in milk.

关 键 词：氨基糖苷 超高效液相色谱-串联质谱法 牛奶 弱阳离子交换固相萃取 残留 

分 类 号：O657.63[理学—分析化学]