药用胶塞常用抗氧剂及可提取硫含量测定方法

Determination of Antioxidants and Extractable Sulfur in Medicinal Rubber Stopper

目的 建立一种高效液相色谱法,以同时检测药用胶塞中多种抗氧剂和可提取硫。方法 采用二氯甲烷作为提取溶剂,微波萃取药用胶塞中的目标化合物,用高效液相色谱法测定目标物的含量。色谱柱为Waters Symmetry RP 18,流动相为乙腈甲醇水,梯度洗脱,检测波长为277 nm。结果 该方法能高效地分离目标化合物,各化合物分离度良好。在0.2~20μg/mL内线性良好,相关系数r≥0.999 3,检测限为0.03~0.09μg/mL,回收率为86.73%~108.91%,相对标准偏差RSD为0.47%~5.68%。通过该种方法测定不同厂家不同批次药用胶塞,结果检出了抗氧剂BHT及其降解物BHT–CHO、BHT–Q,抗氧剂1076和1010及其降解物1310,以及可提取硫。结论 文中建立的高效液相方法准确、简便、灵敏度较高,能够高效快速地测定药用胶塞中常用抗氧剂及其降解产物与可提取硫的含量。

The work aims to establish a high performance liquid chromatography(HPLC) method to detect different antioxidants and extractable sulfur in medicinal rubber plugs simultaneously. Dichloromethane was used as extraction solvent. The target compounds in medicinal rubber plugs were extracted via microwave method. Content of target was tested by the HPLC via gradient elution. Waters Symmetry RP 18 was used as chromatographic column. Acetonitrile, methanol and distilled water were used as mobile phases. The detection wave was set to 277 nm. The target compounds can be separated by HPLC efficiently. The separated products possessed excellent resolution. There was a favourable linearity in the range of 0.2-20 μg/mL with the correlation coefficient r ≥ 0.999 3. The detection limit of this method was 0.03-0.09 μg/mL, the rate of recovery was 86.73%-108.91% and the relative standard deviation(RSD) was 0.47%-5.68%. Medicinal rubber plugs with different batches from different manufacturers were detected by this method.As a results, antioxidant(BHT) and its degradation products(BHT-CHO, BHT-Q), antioxidants(1076 and 1010) and their degradation product(1310), as well as extractable sulfur were detected. The HPLC method established in this work is accurate, convenient and highly sensitive. It can determine the contents of antioxidants and their degradation products and extractable sulfur in common medicinal rubber plugs rapidly and efficiency.