超高效液相色谱-串联质谱联用法同步检测抗生素生产废水中螺旋霉素与新螺旋霉素残留

采用超高效液相色谱-串联质谱法同步测定了抗生素生产废水中残留的螺旋霉素(SPM-Ⅰ)和新螺旋霉素(NSPM-Ⅰ)。考察了萃取溶剂种类、水样pH值、萃取次数、水样与萃取溶剂的体积比等因素对目标物回收率的影响。以ACQUITY UPLC BEH C18(100 mm×2.1 mm i.d.，1.7 μm)为分析柱，0.1%甲酸水溶液和乙腈为流动相梯度淋洗，流速0.2 mL/min，电喷雾正离子多重反应监测模式检测。标准曲线在0.02~1.00 mg/L范围内线性关系良好，r2均大于0.999。方法回收率为70% ~ 88%，相对标准偏差小于10%，检出限(S/N=3)分别为0.03 μg/L(SPM-Ⅰ)和0.06 μg/L(NSPM-Ⅰ)。该方法应用于无锡市某制药厂抗生素生产废水中SPM-Ⅰ和NSPM-Ⅰ的检测，检出质量浓度分别为（115.6±2.7） mg/L和（5.3±0.4） mg/L。

Simultaneous Determination of Spiramycin and Neospiramycin in Antibiotic Production Wastewater by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the simultaneous determination of spiramycin(e.g.spiramycin Ⅰ,SPM-Ⅰ) and neospiramycin(e.g.neospiramycin Ⅰ,NSPM-Ⅰ) residues in antibiotic production wastewater.The factors influencing the recoveries of antibiotics,including organic extractant type,water sample pH value,extraction time and ratio of water sample to organic extractant,were investigated.The target compounds were separated on an ACQUITY UPLC BEH C18 column(100 mm × 2.1 mm i.d.,1.7 μm) by gradient elution using 0.1% formic acid(A) and acetonitrile(B) as mobile phases at a flow rate of 0.2 mL/min.The qualification and quantification of target antibiotics were carried out by MS/MS with positive electrospray ionization under multiple reaction monitoring(MRM) mode.The calibration curves were linear over an antibiotic concentration range of 0.02-1.00 mg/L with correlation coefficients(r2) more than 0.999.The recoveries of antibiotics ranged from 70% to 88% with relative standard deviations(RSD,n=6) less than 10%.The detection limits(S/N=3) for SPM-Ⅰ and NSPM-Ⅰ were 0.03 μg/L and 0.06 μg/L,respectively.The developed method was applied in the determination of antibiotic production wastewater from a pharmaceutical manufacturing factory in Wuxi City,with SPM-Ⅰ of(115.6±2.7) mg/L and NSPM-Ⅰ of(5.3±0.4) mg/L.