摘要
建立了测定西吡氯铵含片中氯代十四烷、氯代十五烷、氯代十六烷、氯代十七烷、氯代十八烷的方法。采用气相色谱-质谱联用法(GC-MS),用HP-5MS毛细管色谱柱,以多反应监测模式(MRM)进行测定。初始柱温为60℃,保持1 min后,以30℃·min^(-1)升温至300℃,保持3 min;进样口温度为350℃;载气为氦气;柱流速1.0 mL·min^(-1);分流比为10∶1;进样量为1μL。待测成分在2.6~26 ng·mL^(-1)内线性关系良好(r>0.9990),定量限浓度分别为0.82,1.27,1.35,3.54和4.39 ng·mL^(-1),回收率分别为101.28%,101.96%,102.02%,101.30%和102.55%,RSD<10.0%。该方法灵敏度高,准确度好,可用于西吡氯铵含片中氯代烷烃类杂质的检测。
To determine 1-chlorotetradecane,1-chloropentadecane,1-chlorohexadceane,1-chloroheptadecane and 1-chloroctadecane in cetylpyridinium chloride buccal tablets,a gas chromatography-mass spectrometry(GC-MS)method was used.The chromatographic column was HP-5MS capillary column.The measurement was performed in multiple reaction monitoring(MRM)mode.The initial colum temperature was 60℃,hold on 1 minute,then raise the temperature to 300℃at the rate of 30℃·min^(-1),hold on 3 minutes.The inlet temperature was 350℃;the carrier gas was helium;the column flow rate was 1.0 mL·min^(-1);the split ratio was 10∶1;the injection volume was 1μL.It was linear for the alkyl chlorides in the range of 2.6~26 ng·mL^(-1).The limits of quantification were 0.82,1.27,1.35,3.54 and 4.39 ng·mL^(-1),respectively,and the recoveries were 101.28%,101.96%,102.02%,101.30%and 102.55%,respectively,with the RSD below 10.0%.The method is sensitive and accurate,and can be used for the determination of 1-Chlorotetradecane,1-Chloropentadecane,1-Chlorohexadceane,1-Chloroheptadecane and 1-Chloroctadecane in cetylpyridinium chloride buccal tablets.
作者
刘延凤
卢红华
孙建合
伊磊
张贵民
Liu Yanfeng;Lu Honghua;Sun Jianhe;Yi Lei;Zhang Guimin(Lunan Pharmaceutical Group Co.,Ltd.,National Chiral Pharmaceuticals Engineering and Technology Research Center,Linyi 273400,China)
出处
《山东化工》
CAS
2023年第17期169-170,180,共3页
Shandong Chemical Industry
关键词
气相色谱-质谱法
西吡氯铵含片
氯代烷烃类杂质
gas chromatography-mass spectrometry
cetylpyridinium chloride buccal tablets
alkyl chlorides
