| 超高效液相色谱串联质谱法同时测定叶菜中13种抗生素 |
| 摘要点击 1500 全文点击 593 投稿时间：2019-07-11 修订日期：2019-09-02 |
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| 中文关键词 超高效液相色谱 质谱 叶菜 抗生素 联合检测方法 |
| 英文关键词 ultra-high performance liquid chromatography mass spectrometry leafy vegetables antibiotics detection methods |
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| 中文摘要 |
| 建立了超高效液相色谱串联三重四极杆质谱（UPLC-MS/MS）同时检测叶菜类蔬菜中磺胺类、喹诺酮类、大环内酯类13种抗生素的分析方法.优化蔬菜基质中抗生素的提取液种类、净化方式、洗脱液种类，以及探讨环境变化和实验条件对实验结果的影响后，确定最优方案为称取500 mg的蔬菜样品，加入20 mL甲醇-Mcllvaine-Na2EDTA溶液，超声和离心提取3次后，旋转蒸发至20 mL过HLB固相萃取柱.以6 mL甲醇洗脱，收集洗脱液，氮吹近干，用乙腈：水（体积比2：8）混合溶液复溶，离心、过滤后采用UPLC-MS/MS进行检测.流动相A相为1‰的甲酸水溶液，B相为乙腈，梯度洗脱.结果显示，小白菜在300 ng·g-1加标时，13种抗生素的加标回收率为38.05%~96.97%，150 ng·g-1时，加标回收率为34.52%~111.10%，50 ng·g-1时，加标回收率为41.75%~107.13%，相对偏差RSD值均小于8.68%.检出限为0.4~1 ng·g-1、定量限为1.5~3 ng·g-1，在不同种类的叶菜上也表现出较好的提取和回收效率，具有较好的分析应用效果.实际的样品检测发现，4种叶菜不同程度地检测出了抗生素的残留.总的含量范围（以干重计）为1.59~32.01ng·g-1.小白菜所含抗生素含量最高，其次为白菜、生菜和芫荽.磺胺二甲基嘧啶为叶菜中含量最高的抗生素种类.各抗生素检测出的含量虽很低，但仍不能忽略长期食用带来的潜在健康风险. |
| 英文摘要 |
| An analytical approach was developed to simultaneously determine 13 antibiotics in sulfonamides, quinolones, and macrolides in leafy vegetables by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS). After optimizing extracted solutions, purification methods, and eluents of antibiotics in vegetable substrates, and taking into account the influence of environmental changes and experimental conditions on the results, the optimal experimental scheme was determined. This involved ①weighing 500 mg of vegetable samples and adding 20 mL of methanol-Mcllvaine-Na2 EDTA solution; ② conducting ultrasonic and centrifugal extraction three times; ③ Allowing rotary evaporation to 20 mL to pass a HLB solid phase extraction column; ④ Eluting the extraction column using 6 mL of methanol, upon which the eluent was dried almost completely; ⑤ Re-dissolving the eluent with a mixed solution of acetonitrile:water (volume ratio of 2:8); ⑥ Detecting by UPLC-MS/MS after centrifugation and filtering. Phase A and B of UPLC-MS/MS used an aqueous solution of 1‰ formic acid and acetonitrile, respectively to conduct gradient elution. Results showed that when the pakchoi spiked at 300 ng·g-1, the spiked recoveries of 13 antibiotics were 38.05%-96.97%. At 150 ng·g-1, the spiked recoveries were 34.52%-111.10%. At 50 ng·g-1, the recoveries of standard addition were 41.75%-107.13%, and the relative deviation (RSD) values were all below 8.68%. The detection limit was 0.4-1 ng·g-1, and the limit of quantification was 1.5-3 ng·g-1. This demonstrated good extraction and recovery efficiency on different types of leafy vegetables, and presented a good analytical application effect. The antibiotic residues were detected in four kinds of leafy vegetables in found in markets. The total content ranged from 1.59 ng·g-1 to 32.01 ng·g-1, and the antibiotic content in samples was calculated by dry weight. The content of antibiotics in pakchoi was the highest, followed by Chinese cabbage, lettuce, and coriander. Among the antibiotics detected, sulfadimidine was the most abundant from the selected leafy vegetables. The content of antibiotics was very low, however the potential health risks caused by long-term consumption could not be ignored. |
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