ASE-GC-MS/MS法测定海产品中苯并(a)芘含量方法的建立
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摘要
建立快速溶剂萃取-气相色谱-三重四级杆串联质谱(GC-MS/MS)法测定海产品中的苯并(a)芘的分析方法。方法利用快速溶剂萃取仪进行提取,以丙酮和乙腈体系(2︰1, V/V)为提取溶剂, GC-MS/MS法进行定性定量分析。结果表明,苯并(a)芘浓度在0.5～20 ng/mL范围内线性关系良好,相关系数为0.999 1;检出限为0.03μg/kg;两种海产品加标回收率(低点0.1μg/kg,中点0.4μg/kg,高点4.0μg/kg)分别为94.9%和90.0%;精密度RSD (n=6)分别为1.39%和1.65%;重复性RSD (n=6)分别为3.83%和3.26%。试验证明,该方法具有前处理简单、分析速度快、检出限低、检测结果准确等优点。
An ASE-GC-MS/MS method for the determination of benzopyrene in marine products was established. In this method, rapid solvent extraction apparatus was used, acetone and acetontrile system(2︰1, V/V) was selected as extracted solution, and samples were tested qualitatively and quantitatively by GC-MS/MS. The result showed that benzopyrene had good linear relationships in the range of 0.5 to 20 ng/mL, with correlation coefficients of 0.991. Detection limits of benzopyrene were 0.03 μg/kg. The recoveries in 2 kinds of marine products were 94.9% and 90.0%(Lower 0.1 μg/kg, middle 0.4 μg/kg and higher 4.0 μg/kg), repectively. The RSD(n=6) of precision was 1.39% and 1.65%, and RSD(n=6) of reproducibility was 3.83%and 3.26%. It is proved that this method is simple pre-treated, rapid analysis, low detection and accuracy.
An ASE-GC-MS/MS method for the determination of benzopyrene in marine products was established. In this method, rapid solvent extraction apparatus was used, acetone and acetontrile system(2︰1, V/V) was selected as extracted solution, and samples were tested qualitatively and quantitatively by GC-MS/MS. The result showed that benzopyrene had good linear relationships in the range of 0.5 to 20 ng/mL, with correlation coefficients of 0.991. Detection limits of benzopyrene were 0.03 μg/kg. The recoveries in 2 kinds of marine products were 94.9% and 90.0%(Lower 0.1 μg/kg, middle 0.4 μg/kg and higher 4.0 μg/kg), repectively. The RSD(n=6) of precision was 1.39% and 1.65%, and RSD(n=6) of reproducibility was 3.83%and 3.26%. It is proved that this method is simple pre-treated, rapid analysis, low detection and accuracy.
引文
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[12]王红青,韩里明,屠海云,等.固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘[J].食品科学, 2012, 33(14):216-218.
[2]沈浥.水产动物及其制品中苯并(a)芘的研究进展和标准化现状[J].食品研究与开发, 2017, 38(21):220-226.
[3]万红丽.烧烤肉制品中3, 4-苯并(a)芘的分析检测与残留变化规律的研究[D].南京:南京农业大学, 2007.
[4]梁涵峪,石晶,丁晓雯,等.市售中式香肠苯并(a)芘来源分析[J].食品工业科技, 2013, 34(17):122-125.
[5]邓燕霞,古盼,刘海龙,等.苯并芘诱导肝脏的炎症损伤及EGFR的表达变化[J].癌变·畸变·突变, 2017, 29(5):383-386.
[6]龙凌云,杨庆懿,邓永琪,等.固相萃取-高效液相色谱法测定食用油中苯并(a)芘[J].农产品加工, 2015, 5(5):44-46.
[7]吴海智,周丛,袁列江,等.高效液相色谱法快速测定植物油中苯并芘的研究[J].安徽农业科技, 2011, 39(10):6075-6076.
[8]弓玉红,郝林,郭凯凯,等.萃取-紫外分光光度法测定土壤中3, 4-苯并芘含量[J].山西农业科技, 2012, 40(4):383-385.
[9]陈雨喆,何强,虞丹尼,等.高铁酸钾降解苯并芘的荧光光谱研究[J].光谱学与光谱分析, 2012, 32(7):1842-1845.
[10]马小杰.大体积全自动固相萃取气相色谱-质谱法测定水中苯并芘[J].化学分析计量, 2015, 24(4):40-43.
[11]刘春波,申钦鹏,张凤梅,等.在线液相-气相二维色谱测定卷烟主流烟气中的苯并(a)芘[J].分析化学, 2016, 44(2):241-246.
[12]王红青,韩里明,屠海云,等.固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘[J].食品科学, 2012, 33(14):216-218.