UPLC检测饲料中恩诺沙星、环丙沙星和沙拉沙星

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恩诺沙星、环丙沙星和沙拉沙星属于化学合成抗菌素类药物,在动物的饲料中添加会减少动物感染肠道类疾病的概率,但是恩诺沙星、环丙沙星和沙拉沙星这类药物却会残留在动物的肌肉组织中,人食用后会给人体健康带来不利影响,对生长发育中的儿童影响尤其不利,细菌耐药和不良反应也相继发生,主要有过敏、溢血和肾衰等不良反应。此外还有可能诱发精神病及癫痫患者发病的风险,增加胎儿畸形的风险。以超高效液相色谱-荧光法(UPLC)检测饲料中的恩诺沙星、环丙沙星和沙拉沙星类违禁药物进行探讨,试样用磷酸盐缓冲溶液提取,C18萃取柱净化,流动相洗脱后,用超高效液相色谱-荧光检测器测定,激发波长280 nm,发射波长450 nm处测定其吸光度,同条件下测定恩诺沙星、环丙沙星和沙拉沙星药物标准品相对应的峰面积响应值,恩诺沙星、环丙沙星和沙拉沙星含量与吸光度值在一定质量浓度范围内成正比,试样与标准品比较定量。经试验,此方法具有操作简单、回收率稳定和检测时间短等优点;标准品峰面积响应值稳定,此方法在环丙沙星、恩诺沙星和沙拉沙星质量浓度为0.1~0.5μg/mL时,能够达到较好线性系数,符合检测时的相关要求;恩诺沙星相关系数r≥0.999 96,环丙沙星相关系数r≥0.999 87,沙拉沙星相关系数r≥0.999 82。恩诺沙星平均回收率为83.5%~96.5%,批内变异系数≤4.2%,批间变异系数≤7.5%;环丙沙星的平均回收率为74.9%~95.5%,批内变异系数≤5.1%,批间变异系数≤7.7%;沙拉沙星平均回收率为80.1%~95.0%,批内变异系数≤4.5%,批间变异系数≤6.5%。 Enrofloxacin, ciprofloxacin, and sarafloxacin are chemically synthesized antibiotics that are added to animal feed to reduce the probability of intestinal infections in animals, but enrofloxacin, ciprofloxacin, and sarafloxacin Star, but these drugs will remain in animal muscle tissue, human consumption will have adverse effects on human health, growth and development of children in particular adverse effects, bacterial resistance and adverse reactions have also occurred, the main allergies, Hemorrhage and renal failure and other adverse reactions. In addition there may be induced psychosis and epilepsy patients the risk of increased risk of fetal malformations. The detection of enrofloxacin, ciprofloxacin and sarafloxacin in bananas by UPLC was carried out. The samples were extracted with phosphate buffered saline, cleaned up with C18 column and flowed Phase eluted with ultra-high performance liquid chromatography - fluorescence detector measured at an excitation wavelength of 280 nm, the emission wavelength was measured at 450 nm absorbance, the same conditions enrofloxacin, ciprofloxacin and sarafloxacin drug standards The corresponding peak area response value, enrofloxacin, ciprofloxacin and sarafloxacin content and absorbance value in a certain range of mass concentration is proportional to the sample compared with the standard quantitative. The method has the advantages of simple operation, stable recovery rate and short detection time; the peak area response value of the standard product is stable; the method has the advantages that in the ciprofloxacin, enrofloxacin and sarafloxacin mass concentrations of 0.1-0.5 μg / mL, the better linearity coefficient can be achieved, which meets the relevant requirements of detection. The correlation coefficient of enrofloxacin is r≥0.999 96, the correlation coefficient of ciprofloxacin is r≥0.99987, and the correlation coefficient of sarafloxacin is r≥0.999 82. The average recoveries of enrofloxacin were 83.5% -96.5%, intra-assay CV of ≤ 4.2%, inter-assay CV of ≤ 7.5%, average recovery of ciprofloxacin of 74.9% -95.5%, intra-assay CV of ≤ The average recovery of sarafloxacin was 80.1% ~ 95.0%, the intra-assay coefficient of variation was 4.5% and the inter-assay coefficient of variation was less than or equal to 6.5%.
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