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    固相萃取-超高效液相色谱-串联质谱法测定水产品中多种兽药的残留量

    UHPLC-MS/MS Determination of Varieties of Veterinary Drug Residues in Aquatic Products with Solid Phase Extraction

    • 摘要: 用乙腈-乙酸乙酯(3+2)混合液(15.0 mL)作溶剂超声提取水产品样品(3.00 g)中喹诺酮(QNL′s)及磺胺(SFM′s)两类兽药的残留物,离心后取10.00 mL清液,用氨基固相萃取柱进行分离。相继用正己烷及乙腈洗去油脂及干扰物质,然后用甲醇和甲醇-乙酸(99+1)的混合液洗脱两类药物的残留。洗脱液在45 ℃蒸干,用乙腈和含0.1%(φ)甲酸的5 mmol·L-1乙酸铵溶液(1+4)的混合液溶解残渣,并定容至1 mL,按仪器工作条件进行气相色谱-质谱分析。以8种药物内标对上述两类兽药共14种进行定量。14种药物的线性范围均在30 μg·kg-1以内,检出限(3S/N)均为1 μg·kg-1。在2种水产品中加入混合标准溶液并按方法进行回收试验,测得回收率在81.2%~116%之间,测定值的相对标准偏差(n=6)在0.72%~9.8%之间。

       

      Abstract: Mixture of acetonitrile and ethyl acetate(3+2) (15.0 mL) was used as solvent in the ultrasonic assisted extraction of varieties of veterinary drug residues attributed to categories of quinolones (QNL′s) and sulfonamides (SFM′s) in sample (3.00 g) of aquatic products. After centrifugation, 10.00 mL of the supernatant were taken for separation using amino-based SPE column. The column was rinsed with n-hexane and acetonitrile in succession to remove fats and interfering substances, and then eluted successivly with methanol and mixture of CH3OH and CH3COOH (99+1), the eluate was collected and evaporated to dryness at 45 ℃. The residue was taken up with 1 mL of a mixture of acetonitrile and 5 mmol·L-1 NH4OAc solution (which contains 0.1% by vol. of formic acid), mixed in the ratio of 1 to 4. The solution was used for LC-MS analysis. 8 drug standards were used as internal standards in the quantification of 14 drugs attributed to QNL′s and SFM′s. Linearity ranges for these drugs were found in the same range within 30 μg·kg-1, with detection limits (3S/N) same as 1 μg·kg-1. Recovery was tested by standard addition method using 2 aquatic product samples as matrixes, results of recovery in the range of 81.2%-116%, and values of RSD′s (n=6) found were ranged from 0.72% to 9.8%.

       

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