| 丁丽玲,鲁晓旭,李银生,邱江平.蚯蚓体内恩诺沙星残留的检测方法研究[J].农业环境科学学报,2016,35(2):403-408. |
| 蚯蚓体内恩诺沙星残留的检测方法研究 |
| A detection method for enrofloxacin residues in earthworms |
| 投稿时间：2015-09-20 |
| DOI：10.11654/jaes.2016.02.027 |
| 中文关键词: 恩诺沙星 蚯蚓 高效液相色谱法 回收率 滤纸染毒 |
| 英文关键词: enrofloxacin earthworm HPLC recovery rate filter paper exposure |
| 基金项目:国家自然科学基金项目(31172360) |
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| 摘要点击次数: 3357 |
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| 中文摘要: |
| 为进一步研究恩诺沙星对蚯蚓的生态毒理,建立了用荧光检测高效液相色谱法测定蚯蚓体内恩诺沙星残留量的检测方法。以0.1 mol·L-1磷酸液(pH12)+乙腈=1+3(V/V)作为提取液,脱脂,浓缩,再用流动相溶解。液相色谱条件:荧光检测器,激发波长280 nm,发射波长450 nm。流动相:0.025 mol·L-1磷酸/三乙胺缓冲液(pH3.0)+乙腈=83+17(V/V)。恩诺沙星标准曲线范围5~500 ng·mL-1,对其进行3种浓度回收率测定,回收率在81%~88%之间,平均回收率为84.5%,变异系数10%以内,恩诺沙星的最低检出限为2 ng·g-1。对蚯蚓进行恩诺沙星滤纸染毒,浓度分别为0.16、1.6、16、32μg·cm-2,每个浓度设置4个平行,对照为不加恩诺沙星的超纯水,48 h后检测各个浓度下蚯蚓体内恩诺沙星的平均含量分别为1.53、16.81、113.32、120.83μg·g-1。可见,蚯蚓对外源恩诺沙星有较好的吸收,但当外源药物浓度达到一定程度后,对恩诺沙星的吸收量将不再无限制增加,且趋于稳定,验证了该测试方法是简单、快速、可行的。 |
| 英文摘要: |
| An assay method using high performance liquid chromatography(HPLC) with fluorescence detection was established to quantify enrofloxacin residues in earthworms. The extraction solution comprised 0.1 mol·L-1 phosphoric acid(pH12)+acetonitrile(1+3,V/V). The initial extracts were defatted, evaporated, and re-dissolved in mobile phase consisting of 0.025 mol·L-1 phosphoric acid/triethylamine buffer(pH3.0)+ acetonitrile(83+17,V/V). The fluorescence detector excitation wavelength was 280 nm, and the emission wavelength 450 nm. The linear range of the standard curve was 5~500 ng·mL-1. The recoveries of 3 concentration groups were between 81% and 88% with an average of 84.5% and the coefficient of variation was less than 10%. The detection limit of enrofloxacin was 2 ng·g-1. Earthworms were exposed to filter papers soaked in enrofloxacin with concentrations of 0, 0.16, 1.6, 16μg·g-1 and 32μg·cm-2, and 4 replicates in each case. After 48 hours of exposure, the average enrofloxacin concentration in earthworms was 0, 1.53, 16.81, 113.32μg·g-1 and 120.83μg·g-1, respectively. These results show that the absorption of enrofloxacin by earthworms increased linearly up to 1.6μg·cm-2 exposure concentration, and then asymptotically to a maximum of approximately 120μg enrofloxacin·g-1 earthworm tissue. |
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