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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Determination of sulfonamides in swine muscle after salting-out assisted liquid extraction with acetonitrile coupled with back-extraction by a water/acetonitrile/dichloromethane ternary component system prior to high-performance liquid chromatography
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Determination of sulfonamides in swine muscle after salting-out assisted liquid extraction with acetonitrile coupled with back-extraction by a water/acetonitrile/dichloromethane ternary component system prior to high-performance liquid chromatography

机译:高效液相色谱法前,通过水/乙腈/二氯甲烷三元组分系统加乙腈盐析辅助液体萃取,然后通过水/乙腈/二氯甲烷三元组分系统反萃取,测定猪肌肉中的磺酰胺

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摘要

A salting-out assisted liquid extraction coupled with back-extraction by a water/acetonitrile/dichloromethane ternary component system combined with high-performance liquid chromatography with diode-array detection (HPLC-DAD) was developed for the extraction and determination of sulfonamides in solid tissue samples. After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, an aliquot of 1 mL of the acetonitrile extract containing a small amount of dichloromethane (250-400 mu L) was alkalinized with diethylamine. The clear organic extract obtained by centrifugation was used as a donor phase and then a small amount of water (40-55 mu L) could be used as an acceptor phase to back-extract the analytes in the water/acetonitrile/dichloromethane ternary component system. In the back-extraction procedure, after mixing and centrifuging, the sedimented phase would be water and could be with drawn easily into a microsyringe and directly injected into the HPLC system. Under the optimal conditions, recoveries were determined for swine muscle fortified at 10 ng/g and quantification was achieved by matrix-matched calibration. The calibration curves of five sulfonamides showed linearity with the coefficient of estimation above 0.998. Relative recoveries for the analytes were all from 96.5 to 109.2% with relative standard deviation of 2.7-4.0%. Preconcentration factors ranged from 16.8 to 30.6 for 1 mL of the acetonitrile extract. Limits of detection ranged from 0.2 to 1.0 ng/g.
机译:开发了一种盐析辅助液体萃取,并结合水/乙腈/二氯甲烷三元组分系统与高效液相色谱-二极管阵列检测(HPLC-DAD)进行反萃取,用于固体中磺酰胺的萃取和测定组织样本。用乙腈将猪肌肉匀浆并用盐促进分配后,用二乙胺将等分试样的1 mL乙腈萃取液(含少量二氯甲烷(250-400μL))进行碱化。通过离心获得的透明有机萃取物用作供体相,然后可以将少量水(40-55μL)用作受体相,以反萃取水/乙腈/二氯甲烷三元组分系统中的分析物。在反萃取过程中,混合和离心后,沉淀的相将是水,可以很容易地吸入微注射器中,然后直接注入HPLC系统中。在最佳条件下,确定了强化浓度为10 ng / g的猪肌肉的回收率,并通过基质匹配校准实现了定量。五种磺酰胺类化合物的校准曲线呈线性关系,估计系数大于0.998。分析物的相对回收率均为96.5%至109.2%,相对标准偏差为2.7-4.0%。 1 mL乙腈提取物的预浓缩系数范围为16.8至30.6。检出限为0.2至1.0 ng / g。

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