SPE-GC/MS外标法测定水产品中4种丁香酚类麻醉剂

建立了固相萃取/气相色谱-质谱法(GC-MS)测定水产品中4种丁香酚类(丁香酚、异丁香酚、甲基丁香酚和甲基异丁香酚)麻醉剂的分析方法。样品采用正己烷-丙酮混合液(3:1,v/v)提取,乙二胺-N-丙基硅烷(PSA)净化,浓缩后再经硅胶固相萃取柱净化,采用GC-MS测定,外标法定量。结果表明:4种丁香酚类麻醉剂在5.0~200 ng/mL范围内均呈现良好线性关系,相关系数均大于0.998,方法检出限(S/N=3)均为3.0 μg/kg,方法定量限(S/N=10)均为10.0 μg/kg。空白水产品样品在0.01、0.05、0.20 mg/kg等3个加标水平时,4种目标物的平均加标回收率为85.7%~102.5%,相对标准偏差(RSD)为3.3%~9.8%。此方法净化效果较好,灵敏度高,适合水产品中4种丁香酚类麻醉剂的定性和定量分析。

Determination of 4 Eugenol Derivatives in Aquatic Products by SPE-GC/MS Analysis

A method for determination of four eugenol derivatives(eugenol,iso-eugenol,methyl eugenol and methyl iso-eugenol)in aquatic products by gas chromatography-mass spectrometry with solid-phase extraction(SPE-GC/MS)was established. The samples were extracted with N-hexane-acetone mixture(3:1,v/v). The extract was cleaned up with silica solid phase extraction column after being purified by PSA and concentrated. The target compounds were detected by GC-MS with SIM mode. The external standard method was applied for quantitative analysis. As a result,The calibration curves of four eugenol derivatives showed good linearity in the range of 5.0~200 ng/mL with correlation coefficients(r)was over 0.998. The limits of detection(LOD)and the limits of qualification(LOQ)were 3.0,10.0 μg/kg,respectively. When the spiked concentrations were 0.01,0.05,0.20 mg/kg,the average recoveries of four target compounds were of 85.7%~102.5% with the relative standard deviations(RSD)of 3.3%~9.8%.This method was suitable for determination of four eugenol derivatives in aquatic products qualitatively and quantitatively with satisfactory purification effect and sensitivity.