高效液相色谱-串联质谱法测定养殖环境沉积物中多肽类抗生素残留量  

Determination of Peptide Antibiotics Residues in Sediment From Aquaculture Environment by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：钱卓真[1,2] 罗冬莲[2] 罗方方[2] 叶玫[2] 汤水粉[2] 

机构地区：[1]厦门大学材料学院,厦门361005 [2]福建省海洋生物增养殖与高值化利用重点实验室,福建省水产研究所,厦门361013

出　　处：《分析化学》2016年第6期870-875,共6页Chinese Journal of Analytical Chemistry

基　　金：国家海洋局海洋公益性行业科研专项(No.201305043-4);福建省省属公益类科研院所基本科研专项(No.2015R1003-7);福建省海洋高新产业发展专项(闽海洋高新[2014]18号);2014年第一批福建省地方标准制修订项目(闽质监标[2014]137号)资助

摘　　要：建立了测定水产养殖环境沉积物中多肽类抗生素残留量的高效液相色谱串联质谱法。沉积物经10 m L甲醇-柠檬酸-Na_2HPO_4溶液（3∶4,V/V）超声提取2次,0.5 g乙二胺四乙酸二钠络合除杂,5 m L甲基异丁基甲酮净化,HLB固相萃取柱进一步富集净化,MGII C18色谱柱分离,0.1%甲酸与0.1%甲酸-乙腈梯度洗脱,ESI＋电离,多反应监测模式（MRM）监测,外标法定量。粘菌素和杆菌肽在10~10000μg/L范围内,维吉尼霉素M1在4~4000μg/L范围内,线性回归系数均大于0.999,方法检出限为2~5μg/kg,方法定量限为4~10μg/kg。在3个浓度添加水平下,多肽类抗生素回收率79.7%~91.6%,相对标准偏差1.9%~10.8%。本方法具有良好的精密度和准确度,灵敏度高,适用范围广。A new method for the determination of peptide antibiotics in sediment from aquaculture environment by high performance liquid chromatography-tandem mass spectrometry was developed. The target analytes in sediments were ultrasonically extracted twice with citrate buffer solution and methol mixture （3∶ 4, V/ V）, followed by complexation with 0. 5 g of Na2 EDTA, purification with 5 mL of methyl isobutyl ketone, and clean-up with HLB-SPE column. The analytes were separated on a MGII C18 column by gradient elution with 0. 1% formaic acid-0. 1% formaic acid acetonitrile as mobile phase, detected in multiple reaction monitoring （MRM） with electrospray ionization （ESI） under positive ion mode, and quantified by external standard method. The calibration curves were linear （R2 〉0. 999） over a concentration range of 10 -10000μg / L for colistin and bacitracin and 4-4000 μg / L for virginiamycin M1 . The limits of detection （S / N = 3） were 5 μg / kg for colistin and bacitracin and 2 μg / kg for virginiamycin M1 . The limits of quantification （S / N=10） was 10 μg / kg for colistin and bacitracin and 4 μg / kg for virginiamycin M1 . At three spiked levels, the recoveries ranged from 79. 7% to 91. 6% （RSD=1. 9% -10. 8% ）, showing high sensitivity, good reproducibility and wide applicability.

关 键 词：高效液相色谱-串联质谱法 水产养殖环境 沉积物 多肽类药物 残留 

分 类 号：X830[环境科学与工程—环境工程] O657.63[理学—分析化学]