目的: 建立HPLC法测定不同硫化体系橡胶塞中硫化剂和促进剂的含量。方法: 采用Waters SunFire C18(250 mm×4.6 mm,5 μm)色谱柱,以甲醇-水为流动相,进行梯度洗脱,流速1.0 mL·min-1,柱温35 ℃,检测波长220 nm,进样体积10 μL,外标法定量。结果: 14种成分在不同的浓度范围(0.10~20、0.50~20、1.0~20 μg·mL-1)内线性关系良好(r=0.995 9~1.000);方法的精密度、重复性均小于2.0%,供试品溶液在48 h内稳定。不同硫化体系样品的平均回收率为90.0%~108.7%,RSD(n=6)为0.10%~2.8%。从试验结果来看,胶塞中S普遍存在,含量在0.003 0~0.211 4 mg·g-1之间,可见硫磺体系目前仍是主要的硫化体系;3批胶塞中检测出N-环己基-2-苯并噻唑次磺酰胺(CZ)(0.070 8、0.144 3、0.431 2 mg·g-1),1批胶塞中检测出一硫化四甲基秋兰姆(TMTM)(0.099 1 mg·g-1),表明秋兰姆类等会产生有害物质的促进剂几乎无添加。结论: 本方法操作简单,具有较好的精密度和回收率,适用于不同硫化体系硫化剂和促进剂的含量测定,可为胶塞的安全性检测提供参考。
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