Determination of Vulcanizing Agents and Accelerators in Pharmaceutical Rubber Stoppers by Headspace Gas Chromatography-Sulfur Chemiluminescence Detector
10.3870/j.issn.1004-0781.2025.04.008
- VernacularTitle:顶空气相色谱-硫化学发光检测器法测定药用胶塞中硫化剂及硫化促进剂
- Author:
Qian GU
1
;
Yuanliang WANG
;
Xiaowu XIAO
;
Xia ZHAO
;
Bijun ZHU
;
Bilin ZHU
Author Information
1. 江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌 330029;江西中医药大学药学院,南昌 330004
- Publication Type:Journal Article
- Keywords:
Medical rubber stopper;
Sulfur chemiluminescence detector;
Vulcanizing agent;
Vulcanizing accelerator
- From:
Herald of Medicine
2025;44(4):547-553
- CountryChina
- Language:Chinese
-
Abstract:
Objective The aim of this study was to develop a method for the determination of nine vulcanizing agents and accelerators in pharmaceutical rubber stoppers by headspace gas chromatography with sulfur chemiluminescence detector(HS-GC-SCD).Methods A DB-1 capillary column(30 m×0.32 mm×0.25 μm)was used with He as the carrier gas.The injection port temperature was 220 ℃,the split ratio was 10∶1,and the carrier gas flow rate was 1.5 mL·min-1.The temperature program was as follows:the starting temperature was 40 ℃,and it was increased to 60 ℃ at a rate of 5 ℃ per minute,and then to 260 ℃ at a rate of 15℃per minute.SCD detector parameters:base temperature was 280℃,combustion chamber temperature was 800 ℃,air flow rate was 60 mL·min-1,and hydrogen flow rate was 40 mL·min-1.Results The sample pretreatment method was simple and convenient,and it effectively reduced the extraction loss.The methodological results showed that all sulfides showed good linear relationships within the concentration range(r2≥ 0.990).The RSD was less than 2％;and the average recovery rate was 86.4％-97.5％.From the analysis of the sample test results,free sulfur is commonly found in rubber stoppers.Among all the samples of the vulcanization system,the free sulfur detected in the sulfur vulcanization system is higher than the free sulfur produced by degradation of other vulcanization systems.Conclusions This method is simple to operate,compared with other existing detection methods.HS-GC-SCD has a smaller matrix effect,higher sensitivity and selectivity,and is appropriate for quantifying the concentrations of sulfide present in various rubber stoppers.
