多壁碳纳米管净化-超高效液相色谱-质谱法测定水产品中头孢菌素残留量

发布时间：2018-02-03 13:14

本文关键词： 多壁碳纳米管超高效液相色谱-质谱法水产品头孢菌素　出处：《分析化学》2017年03期 　论文类型：期刊论文

【摘要】：建立了水产品可食部位中头孢哌酮、头孢喹肟、头孢洛宁、头孢唑啉、头孢匹林、头孢噻呋、头孢匹罗和头孢氨苄8种头孢菌素的超高效液相色谱-质谱测定法。样品经乙腈-水溶液提取、多壁碳纳米管固相萃取净化后,以Acquity Xselect CSH C_(18)柱为分离柱,用乙腈和0.1%甲酸溶液进行梯度洗脱,电喷雾正离子多反应模式监测。结果表明,8种头孢菌素均呈良好的线性关系(R~2≥0.995),定量限(S/N=10)在2~10μg/kg之间;在阴性样品采取梯度加标,添加回收率为67.3%~94.2%,RSD为3.3%~14%。本方法检测成本低、准确度高、精密度好,能够满足水产品中头孢菌素检测的要求。
[Abstract]:Cefoperazone, cefequinoxime, cefronine, cefazolin, cefpiline and cefotioxime in edible parts of aquatic products were established. Determination of 8 cephalosporins of cefpirosine and cefalexin by ultra-high performance liquid chromatography-mass spectrometry. The samples were extracted by acetonitrile-aqueous solution and purified by solid phase extraction with multi-walled carbon nanotubes (MCNTs). The Acquity Xselect CSH Che _ (18) column was used as the separation column, and the gradient elution was carried out with acetonitrile and 0.1% formic acid solution. The results showed that the linear relationship of 8 cephalosporins was between 0.995g / kg and 0.995g / kg, and the quantitative limit of S / N was 10 渭 g 路kg ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1). The gradient standard was used in the negative samples, and the recovery rate was 67.3%. The RSD was 3.30.The detection cost of this method was low, the accuracy was high and the precision was good. It can meet the requirements of cephalosporin detection in aquatic products.
【作者单位】：浙江省海洋水产研究所浙江省海水增养殖重点实验室;
【基金】：浙江省科技厅计划项目(Nos.2016C32074,2016F30022)资助~~
【分类号】：TS254.7;O657.63
【正文快照】： 1引言头孢菌素又称先锋霉素,是分子中含有头孢烯的β-内酰胺类半合成抗生素[1],具有广谱抗菌作用,临床上主要用于治疗革兰氏菌引起的感染,在动物养殖业中广泛用于治疗畜禽动物尿道、胃肠道和呼吸道感染[2]。动物产品因过量使用头孢菌素造成的残留会通过食物链传递给食用者,引

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