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    超高效液相色谱-串联质谱法测定橡胶产品中5种秋兰姆类硫化促进剂

    UPLC-MS/MS Determination of 5 Thiurams Vulcanization Accelerators in Rubber Products

    • 摘要: 采用超高效液相色谱-串联质谱法测定橡胶产品中的5种秋兰姆类硫化促进剂-二硫化四丁基秋兰姆(TBTD)、二硫化二异丁基秋兰姆(TIBTD)、二硫化四乙基秋兰姆(TETD)、一硫化四甲基秋兰姆(TMTM)和二硫化四甲基秋兰姆(TMTD)。样品经甲醇两次超声提取,提取液在ACQUITY UPLC BEH C18反相色谱柱上分离,以甲醇-水(9+1)混合液作为流动相进行洗脱,质谱分析选择电喷雾离子源和多反应监测模式。5种秋兰姆类硫化促进剂的质量浓度在0.020~1.00 mg·L-1范围内呈线性,TBTD、TIBTD、TETD、TMTM和TMTD的检出限(3S/N)分别为0.004,0.003,0.001,0.005,0.001 mg·L-1,测定下限分别为0.30,0.25,0.075,0.40,0.10 mg·kg-1。加标回收率在81.4%~103%之间,测定值的相对标准偏差(n=5)在4.2%~7.3%之间。

       

      Abstract: UPLC-MS/MS was applied to the determination of 5 thiurams vulcanization accelerators, including tetrabutyl thiuram disulfide(TBTD), tetra(isobutyl)thioperoxydicarbamicacid (TIBTD), disulfiram (TETD), tetramethyl thiuram monosulfide (TMTM) and tetramethylthiuram disulfide(TMTD), in rubber products. The sample was extracted twice with methanol by ultrasonic, and the target compounds in the extract solution were separated on an ACQUITY UPLC BEH C18 reversed-phase column with a mixture of methanol and water as mobile phase. ESI and MRM were adopted in MS analysis. The linearity range of the 5 compound was 0.020-1.00 mg·L-1. The detection limits (3S/N) of TBTD, TIBTD, TETD, TMTM and TMTD were 0.004, 0.003, 0.001, 0.005, 0.001 mg·L-1, respectively, and the lower limits of determination were 0.30, 0.25, 0.075, 0.40, 0.10 mg·kg-1, respectively. Recovery rates obtained by standard addition method were in the range of 81.4%-103%, with RSDs (n=5) in the range of 4.2%-7.3%.

       

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