GC-MS法测定盐酸金霉素眼膏中16种多环芳烃含量
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摘要
目的建立盐酸金霉素眼膏中16种多环芳烃(PAHs)的气相色谱-质谱含量测定方法。方法盐酸金霉素眼膏经正己烷溶解后,用正己烷饱和乙腈多次萃取,浓缩后经GC-MS法检测,气相色谱采用DB-5MS毛细管柱,程序升温,进样口温度250℃,质谱采用电子轰击(EI)离子源,以选择反应监测(SIM)模式进行检测。同时从辅料来源及生产工艺上分析制剂中PAHs异常的主要原因。结果 16种PAHs在相应浓度范围内线性关系良好,定量限(LOQ)为0.3～20.0ng/mL,回收率为72%～118%,相对标准偏差(RSD)均小于2.5%,辅料凡士林的质量直接影响制剂的好坏。结论本法准确度高、灵敏度强,适用于盐酸金霉素眼膏中PAHs的检测,可为眼膏剂的质量控制与安全性评估提供数据参考。
Objective To establish a method for the determination of 16 polycyclic aromatic hydrocarbons(PAHs) in chlortetracycline hydrochloride eye ointment by gas chromatography-mass spectrometry. Methods Chlortetracycline hydrochloride eye ointment was dissolved in n-hexane and extracted by acetonitrile saturated with n-hexane for many times. After concentration, it was detected by GC-MS. GC analysis was performed on the DB-5 MS capillary column with the inlet temperature at 250℃ and the programmed column temperature was used.Mass spectrometry was analyzed under the selective reaction monitoring(SIM) mode by electron bombardment(EI) ion source. In addition, the main causes of PAHs abnormality were studied from the source of excipients and the technological process of production. Results The linear relationships of all compounds were good with the corresponding concentration range, the limits of quantitation(LOQs) of PAHs were 0.3～20.0 ng/mL. The recoveries were found to be from 72% to 118% with relative standard deviation(RSD) lower than 2.5%. The quality of vaseline directly affected the quality of the preparation. Conclusion This method is accurate and sensitive, and is suitable for the detection of PAHs in chlortetracycline hydrochloride eye ointment. This study can provide a data reference for the quality control and safety assessment of eye ointment.
Objective To establish a method for the determination of 16 polycyclic aromatic hydrocarbons(PAHs) in chlortetracycline hydrochloride eye ointment by gas chromatography-mass spectrometry. Methods Chlortetracycline hydrochloride eye ointment was dissolved in n-hexane and extracted by acetonitrile saturated with n-hexane for many times. After concentration, it was detected by GC-MS. GC analysis was performed on the DB-5 MS capillary column with the inlet temperature at 250℃ and the programmed column temperature was used.Mass spectrometry was analyzed under the selective reaction monitoring(SIM) mode by electron bombardment(EI) ion source. In addition, the main causes of PAHs abnormality were studied from the source of excipients and the technological process of production. Results The linear relationships of all compounds were good with the corresponding concentration range, the limits of quantitation(LOQs) of PAHs were 0.3～20.0 ng/mL. The recoveries were found to be from 72% to 118% with relative standard deviation(RSD) lower than 2.5%. The quality of vaseline directly affected the quality of the preparation. Conclusion This method is accurate and sensitive, and is suitable for the detection of PAHs in chlortetracycline hydrochloride eye ointment. This study can provide a data reference for the quality control and safety assessment of eye ointment.
引文
[1]United States Environmental Protection Agency.Method610:Polynuclear Aromatic Hydrocarbons[S].1982:Appendix A to part 136.
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[2]高剑琴,董栋.多环芳烃含量限制法规及测试方法比较[J].橡胶科技,2015,13(7):43-51.
[3]European Council.Directive 2005/69/EC of the European parliament and of the council of 16 November 2005amending for the 27th time council directive 76/769/EEC on the approximation of the laws,regulations and administrative provisions of the member states relating to restrictions on the marketing and use of certain dangerous substances and preparations(polycyclic aromatic hydrocarbons in extender oils and ryres)[Z].Germany:Official Journal of European Union,2005.
[4]European Union.Regultaion(EC)No 1907/2006 of the European parliament and of the council of 18 December2006 concerning the registration,evaluation,authorization and restriction of chemicals(REACH),establishing a European chemicals agency,amending directive 1999/45/EC and repealing council regulation(EEC)No 793/93 and commission regulation(EC)No 1488/94 as well as council directive 76/769/EEC and commission directives 91/155/EEC,93/67/EEC,93/105/EC and 2000/21/E[Z].Germany:Official Journal of European Union,2006.
[5]Zentralstelle Der L?nder Für Sicherheitstechnik.Zek01.4-08,Testing and evaluation of polycyclic aromatic hydrocarbons(PAH)in the GS-mark certification[S].Germany:The Board for Technical work Equipment and Consumer Products,2011.
[6]Product Safety Commission.Testing and assessment of polycyclic aromatic hydrocarbons(PAHs)in the course of awarding the GS mark-Specification pursuant to article 21(1)no.3 of the Product Safety Act(ProdSG)-AfPS GS 2014:01PAK[S].Germany:Federal Institute for Occupational Safety and Health,2014.