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    固相萃取-超高效液相色谱-串联质谱法同时测定环境水体中10种大环内酯类抗生素的含量

    Simultaneous Determination of 10 Macrolide Antibiotics in Environmental Water Bodies by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction

    • 摘要: 通过优化样品保存、前处理、仪器工作条件,提出题示方法测定环境水体中脱水红霉素、罗红霉素、螺旋霉素、吉他霉素、克拉霉素、竹桃霉素、阿奇霉素,泰乐霉素、替米考星、交沙霉素等10种大环内酯类抗生素的含量。取1.0 L水样,添加50 mL甲醇,用0.45 μm玻璃纤维滤膜抽滤,收集滤液,于4 ℃保存,2 d内完成测定。分取500 mL水样,用50%(体积分数)盐酸溶液调节水样酸度至pH 2.0~3.0,加入25 μL 2 mg·L−1阿奇霉素-d3、罗红霉素-d7的混合替代内标溶液和25 mL乙醇,混合均匀。取500 mL处理好的水样以流量5~10 mL·min−1过活化好的HLB固相萃取柱。用5 mL水淋洗,并用氮气吹扫柱子30 min,再依次用5 mL甲醇、5 mL含0.1%(体积分数)甲酸的甲醇溶液在2 mL·min−1流量下洗脱柱子。收集洗脱液,于35 ℃氮吹至近干,加入2 mg·L−1克拉霉素-d3内标溶液25.0 μL,用体积比80∶20的0.05%(体积分数,下同)甲酸溶液和乙腈的混合溶液稀释至1.0 mL,经0.22 μm有机滤膜过滤后采用超高效液相色谱-串联质谱法测定。在色谱分析中,以Eclipse Plus C18色谱柱作为固定相,不同体积比的0.05%甲酸溶液和乙腈的混合溶液作为流动相进行梯度洗脱;在质谱分析中,以电喷雾离子源正离子模式电离,多反应监测模式检测,内标法定量。结果显示:10种目标物的线性范围均为1.0~100 μg·L−1,检出限(3.143s)为0.4~1.0 ng·L−1;按照标准加入法进行回收试验,回收率为58.4%~100%,测定值的相对标准偏差(n=6)为3.2%~20%。方法用于不同来源环境水体的分析,均检出了大环内酯类抗生素,检出量不超过140 ng·L−1

       

      Abstract: By optimizing sample preservation, pretreatment, and instrument working conditions, the method mentioned by the title was proposed to determine 10 macrolide antibiotics in the environmental water body, including erythromycin dehydrate, roxithromycin, spiramycin, kitasamycin, clarithromycin, oleandomycin, azithromycin, tylosin, tilmicosin, and josamycin. The 1.0 L of water sample was taken, and 50 mL of methanol was added. The sample was passed through a 0.45 μm glass fiber filter membrane, and the filtrate was collected and stored at 4 ℃, with the determination completed within 2 d. An aliquot (500 mL) of the water sample was taken, and its acidity was adjusted to pH 2.0-3.0 using a 50% (volume fraction) hydrochloric acid solution. Then, 25 μL of the mixed surrogated internal standard solution containing 2 mg · L-1 azithromycin-d3 and roxithromycin-d7 and 25 mL of methanol were added, and the solution obtained was mixed well. The 500 mL of the treated water sample was passed through an activated HLB solid phase extraction column at a flow rate of 5-10 mL·min-1.The column was rinsed with 5 mL of water and purged with nitrogen for 30 min. Subsequently, the column was eluted sequentially with 5 mL of methanol and 5 mL of a methanol solution containing 0.1% (volume fraction) formic acid at a flow rate of 2 mL·min-1. Then, the eluate was collected, and evaporated to near dryness at 35 ℃ by nitrogen, and then 25.0 μL of the 2 mg·L-1 clarithromycin-d3 internal standard solution was added. The solution was diluted to 1.0 mL with a mixed solution of 0.05% (volume fraction, the same below) formic acid solution and acetonitrile at a volume ratio of 80∶20, and the solution obtained was passed through a 0.22 μm organic filter membrane. The filtrate was analyzed using ultra-high performance liquid chromatography-tandem mass spectrometry. In the chromatographic analysis, a Eclipse Plus C18 column was used as the stationary phase, and gradient elution was performed using mixed solutions composed of 0.05% formic acid solution and acetonitrile at different volume ratios as the mobile phase. In the mass spectrometry analysis, ionization was carried out in positive ion mode with an electrospray ion source, detection was performed in multiple reaction monitoring (MRM) mode, and quantification was achieved using the internal standard method. It was shown that the linear range for 10 target compounds was 1.0-100 μg · L-1, with detection limits (3.143s) in the range of 0.4-1.0 ng · L-1. Test for recovery was conducted using the standard addition method, giving recoveries in the range of 58.4%-100%, and RSDs (n=6) of the determined values ranged from 3.2% to 20%. The proposed method was applied to the analysis of environmental water bodies from different sources, and macrolide antibiotics were detected in all samples, with detection amounts not exceeding 140 ng · L-1.

       

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