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    超高效液相色谱法测定橡胶中6种橡胶助剂的含量

    Determination of 6 Rubber Additives in Rubber by UPLC

    • 摘要: 取条状橡胶样品(厚约2 mm,宽约1 mm)1.000 g,加入体积比为6:1的乙腈-二氯甲烷混合溶液50 mL,超声提取60 min,所得溶液经0.45 μm滤膜过滤,滤液用于超高效液相色谱法分析。用ZORBAX Eclipse XDB-C18色谱柱(4.6 mm×100 mm,1.8 μm)为固定相,以体积比为40:60的乙腈-pH 4.0的12.5 mmol·L-1磷酸二氢钠混合溶液为流动相进行等度洗脱,使所测定的6种橡胶助剂得以分离,对6种橡胶助剂在不同波长处进行紫外检测,防老剂6PPDN-(1,3-二甲基)丁基-N'-苯基对苯二胺的检测波长为290 nm,防焦剂CTP (N-环己基硫代邻苯二甲酰亚胺)和其他4种硫化促进剂TBBS (N-叔丁基-2-苯并噻唑次磺酰胺)、MBTS (2,2-二硫化二苯并噻唑)、CBS (N-环己基-2-苯并噻唑次磺酰胺)、DCBS (N,N-二环己基-2-苯并噻唑次磺酰胺)的检测波长均为226 nm。6种橡胶助剂的标准曲线的线性范围均为5.0~500.0 mg·L-1,其检出限(3S/N)为0.3~2.5 mg·L-1。按标准加入法进行回收试验,测得回收率为82.8%~107%,测定值的相对标准偏差(n=5)均小于5.0%。

       

      Abstract: Rubber sample strips (thickness:ca. 2 mm, width:ca. 1 mm) of 1.000 g were taken and extracted ultrasonically with 50 mL of a mixed solution of CH3CN and CH2Cl2 with the volume ratio of 6:1 for 60 min. The solution was filtered through 0.45 μm filtering membrane and the filtrate was used for UPLC analysis. ZORBAX Eclipse XDB-C18 column (4.6 mm×100 mm, 1.8 μm) was used as stationary phase, and a mixed solution of CH3CN and 12.5 mmol·L-1 NaH2PO4 (pH 4.0) with the volume ratio of 40:60 was used as mobile phase in isogradient elution, in the course of which the 6 rubber additivesi.e., the anti-aging agent 6PPD (N-(1,3-dimethylbuty)-N'-phenyl-phenylenediamine), the anti-charring agnet CTP (N-cyclohexylthiophthalimide) and 4 vulcanizing agents TBBS (N-tert-butyl-2-benzothiazole), MBTS (2,2-dibenzothiazole disulfide), CBS (N-cyclohexyl-2-benzothiazole sulfenamide) and DCBS (N,N-dicyclohexyl-2-benzothiazole sulfenamide) were separated and their absorbances measured spectrophotometrically at different wavelengths of 290 nm (for 6PPD) and of 226 nm (for the remainder). Linearity ranges of the standard curves of the 6 rubber additives were found same between 5.0 mg·L-1 and 500.0 mg·L-1; their detection limits (3S/N) were found in the range of 0.3-2.5 mg·L-1. Test for recovery was made by standard addition method, giving recoveries ranged from 82.8% to 107%. Values of RSDs (n=5) were found all less than 5.0%.

       

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