HPLC—MS／MS法测定水产品中硫酸粘菌素、杆菌肽及维吉尼霉素M1的残留量

建立了水产品中硫酸粘菌素（CS）、杆菌肽（BTC）及维吉尼霉素M1（VBGMM1）3种多肽类抗生素残留量检测的HPLC-MS/MS法.样品经水溶液V（甲醇）∶V（0.1％甲酸水溶液）=2∶5]提取,4％三氯乙酸乙腈除蛋白,乙腈饱和正己烷除脂,过OASIS HLB（60 mg）小柱净化后,利用HPLC-MS/MS法,以选择反应监测模式检测,外标法进行定量分析.CS和BTC在0.01～10.00 mg·L^-1质量浓度范围内线性良好,VGMM1在0.002～2.000 mg·L^-1质量浓度范围内线性良好,R2均大于0.995;3种多肽类抗生素的检出限分别为CS 10 μg· kg^-1、BTC 10 μg·kg^-1、VGMM1 2μg·kg^-1,定量限分别为20 μg ·kg^-1、20 μg ·kg-和4 μg·kg-;选择3个不同浓度水平做加标回收,平均回收率在72.3％ ～ 103.9％,相对标准偏差为1.10％～10.92％.该方法具有操作简便、准确性高、灵敏度高和重现性好等优点,可为检测水产品中这3种药物的残留提供相关技术支持.

Determination of colistin sulfate, bacitracin and virginiamycin M1 residues in aquatic products by HPLC-MS/MS

A high performance liquid chromatography tandem mass spectrometric （HPLC-MS/MS） method was established to simulta- neously detect colistin sulfuric （CS） , bacitraein （BTC） and virginiamyein M1 （VGMM1 ） in aquatic products. We extracted the samples with methanol-O. 1% formieaeid（ V ： V = 2 ： 5 ）, removed their protein with 4% TCA acetonitril, removed fat with acetonitrile saturated n-hexane, and then cleaned them up with OASIS HLB solid phase extraction （SPE） column. Next, we detected the analytes by HPLC-MS/MS under the selected reaction monitoring mode and quantified them by external standard method. Results show that CS and BTC have good linearity between the peak areas in concentrations ranged 0. 01 - 10. 00 mg.L^-1, VGMM1 as well in concentrations ranged 0. 002 -2. 000 mg.L^-1 , and the correlation coefficients （R2） are all more than 0. 995. The detection limits of CS, BTC and VGMM1 are 10 μg.kg^-1, 10 μg.kg-land 2 μg.kg^-1 respectively, and the quantification limits are 20 μg.kg^-1 , 20 μg.kg^-1 and 4 μg.kg-lrespectively. Three samples in three different concentration levels are chosen for recovery, getting a 72. 3% - 103.9% average recovery rate, and a relative standard deviations varying from 1.10% - 10. 92%. In conclusion, method proposed has advantages of simplicity, sensitivity and repeatability, which provide technical support for the detection of these 3 kinds of drug residues in aquatic products.