摘要
目的建立药用橡胶塞中17种多环芳烃的气相色谱-串联质谱测定方法,评估其残留多环芳烃的安全性。方法采用丙酮/正己烷(V丙酮∶V正己烷=1∶1)作为提取溶剂,微波萃取胶塞中目标物,以D8-萘、D10-芘、D12-苯并[a]芘为内标进行定量分析。结果该方法在2~200 ng/mL线性良好,相关系数R为0.9984~0.9999,方法检出限范围为0.35~1.25 ng/g,回收率为92.24%~118.47%,测定结果的相对标准偏差为0.86%~13.23%。采用上述方法对市场上8个厂家的17批胶塞进行提取,其中均提取出不同多环芳烃,致癌性多环芳烃检出量为0.0004~0.1278μg/g;3批胶塞检出苯并[α]芘量为0.0013~0.0042μg/g;非明确致癌性多环芳烃检出量为0.0004~0.2980μg/g。结论该方法准确、灵敏、简便,可用于定量测定胶塞中残留的高风险致癌性多环芳烃(五环以上)。
This paper developed determination methodology of gas chromatography-tandem mass spectrometry for 17 polycyclic aromatic hydrocarbons of pharmaceutical rubber stoppers to evaluate the safety of residual polycyclic aromatic hydrocarbons.A mixture of acetone-hexane(V丙酮∶V正己烷=1∶1)was used as the extraction solvent,the target substances of rubber stopper were extracted by microwave,and D8-naphthalene,D10-pyrene and D12-benzo[a]pyrene were used as internal standards for quantification analysis.Good linearity was observed within the range of 2-200 ng/mL,the correla-tion coefficient R was 0.9984-0.9999,and the limit of detection was in the range of 0.35-1.25 ng/g in this methodology.Besides,the recovery ranged from 92.24%to 118.47%(RSD:0.86%-13.23%).The above method was used to extract 17 batches of rubber stoppers from 8 manufacturers on the market,and different polycyclic aromatic hydrocarbons were extracted from them.The detected amount of carcinogenic PAHs was in the range of 0.0004 to 0.1278μg/g,ben-zo[α]pyrene from 3 batches of the rubber stoppers were in the range of 0.0013-0.0042μg/g and the detected amount of unclear carcinogenic PAHs was 0.0004-0.2980μg/g.This method is accurate,sensitive,simple and suitable for the quan-titative determination of the residual high-risk carcinogenic polycyclic aromatic hydrocarbons(above five rings)in rubber stoppers.
作者
张罗红
黄婉莎
张欣
江燕
ZHANG Luo-hong;HUANG Wan-sha;ZHANG Xin;JIANG Yan(Sichuan Institute for Food and Drug Control,Chengdu 610000,China)
出处
《包装工程》
CAS
北大核心
2021年第17期10-19,共10页
Packaging Engineering
基金
四川省食品药品检验检测院科研项目(2019-KYYL-012)。
关键词
多环芳烃
微波萃取
药用胶塞
可提取物
气相色谱-串联质谱
polycyclic aromatic hydrocarbons
microwave extraction
pharmaceutical rubber stoppers
extractable substances
gas chromatography-tandem mass spectrometry
