| 液相色谱-串联质谱法测定养殖水体中的氯霉素 |
| Determination of Chloramphenicol Level in Aquaculture Water by Liquid Chromatography-Tandem Mass Spectrometry |
| 投稿时间：2015-06-10 修订日期：2015-11-06 |
| DOI：10.15928/j.1674-3075.2015.06.003 |
| 中文关键词:氯霉素 养殖水体 液相色谱-串联质谱法 |
| 英文关键词:chloramphenicol aquaculture water liquid chromatography-tandem mass spectrometry |
| 基金项目:辽宁省地方标准资助项目（2014333） |
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| 中文摘要: |
| 本文采用回收率较高、较稳定的内标定量法（对养殖水体中氯霉素的检测方法进行了研究, 建立了养殖水体中氯霉素残留的检测方法。应用液相色谱-串联质谱（LC-MS/MS）测定养殖水体中氯霉素的含量，量取250 mL水样，用100 mL乙酸乙酯分2次萃取，萃取液经旋转蒸发仪浓缩近干，以40%的甲醇-水溶液定容至1 mL。氯霉素标准系列溶液浓度为0.25、0.50、1.00、1.25、2.50、5.00 ng/mL，氘代氯霉素的含量均为2.0 ng/mL，上机检测，内标法定量。结果表明，氯霉素为外标，氘代氯霉素为内标，其峰面积比值（y）与浓度比值（x）的曲线方程为：y=1.136512x+0.012050（R2＝0.9990）；该方法氯霉素的检出限为2 ng/L，定量限为4 ng/L，仪器线性范围为0.25～5.0 ng/mL；加标浓度在2～20 ng/L时，平均回收率在80%～110%，相对标准偏差小于10%。实验证明该方法比较稳定、灵敏度高，适用于检测养殖水体中氯霉素的含量。 |
| 英文摘要: |
| Chloramphenicol is forbidden as a drug for veterinary use in China because of toxicity and serious side effects to humans. However, chloramphenicol is often determined in routine monitoring for drug residues in water-based products, natural waters and even in the ponds of some restaurants. Thus, it is important to develop a reliable method for determining chloramphenicol in water to support monitoring, control sources of chloramphenicol and improve the detection index of pollution-free water. In this study, a high performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method was developed to determine chloramphenicol levels in aquaculture water. Water samples were obtained from the aquafarm， seedling rearing rooms and storage ponds of restaurants. A 250 mL water sample was extracted with 100 mL of ethyl acetate twice, each for three minutes and the extractant was concentrated to 1 mL prior to analysis. The analysis was carried out in the multi-reaction monitoring (MRM) mode and the internal standard isotope dilution method was used for chloramphenicol quantification. The sensitivity and accuracy of the method was tested using a series of low concentration chloramphenicol standards (0.25, 0.50, 1.00, 1.25, 2.50 and 5.00 ng/mL), all with cekafix as the internal standard at a concentration of 2.0 ng/mL. The calibration curve for chloramphenicol exhibited good linearity over the concentration range from 0.25 ng/mL to 5.0 ng/mL, with detection limit of 2 ng/L and quantification limit of 4 ng/L. When the standard addition concentration was in the range of 2-20 ng/L, the average recovery rate was in the range of 80%-110% and the relative standard deviation (RSD) was less than 10%. The method proved to be accurate, stable and sensitive and meets the requirements for chloramphenicol detection in aquaculture water. |
| 张秀妍,马琳.2015.液相色谱-串联质谱法测定养殖水体中的氯霉素[J].水生态学杂志,36(6):14-18. |
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