ICP-MS法测定辅酶Q_(10)原料及制剂中22种元素杂质
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摘要
目的:建立测定辅酶Q_(10)原料及制剂中22种元素杂质的方法。方法:以密闭高压微波消解技术处理样品,采用电感耦合等离子体质谱法以全定量的方式测定镉(Cd)、铅(Pb)、砷(As)、汞(Hg)、钴(Co)、钒(V)、镍(Ni)的含量,以半定量的方式测定其余15种元素杂质的含量。结果:辅酶Q_(10)中Cd、Pb、As、Hg、Co、V、Ni的加样回收率为89.8%～103.5%,检测下限均满足测定要求。辅酶Q_(10)原料所含元素杂质均远低于限度值,企业1～3生产的辅酶Q_(10)胶囊含Pb浓度较高。企业3、14生产的辅酶Q_(10)胶囊含(Al)浓度较高,有可能是药用辅料滑石粉引入。结论:所用方法准确快捷,灵敏度高,适用于辅酶Q_(10)原料和制剂中元素杂质的测定。
Objective:To establish a method for determination of twenty-two elemental impurities in coenzyme Q_(10) material and preparations. Methods:A rapid method was established based on microwave digestion assisted with inductively coupled plasma-mass spectrometer(ICP-MS)for full quantitative analysis for Cd,Pb,As,Hg,Co,V,Ni and semi quantitative analysis for other 15 elemental impurities. Results:The recoveries of Cd,Pb,As,Hg,Co,V,Ni in coenzyme Q_(10) were 89.8%-103.5%,and the limits of detection all met the requirements of determination. The elemental impurities in coenzyme Q_(10) material were far below limits. The concentrations of lead in coenzyme Q_(10) capsules made by manufacturers 1-3 were higher than the other. The higher concentration of aluminum in coenzyme Q_(10) capsules made by manufacturers 3 and 14 were supposed come from pharmaceutical excipient talc. Conclusion:The proposed method is accurate,rapid,and sensitive,which can be applied to the determination of elemental impurities in coenzyme Q_(10) material and preparations.
Objective:To establish a method for determination of twenty-two elemental impurities in coenzyme Q_(10) material and preparations. Methods:A rapid method was established based on microwave digestion assisted with inductively coupled plasma-mass spectrometer(ICP-MS)for full quantitative analysis for Cd,Pb,As,Hg,Co,V,Ni and semi quantitative analysis for other 15 elemental impurities. Results:The recoveries of Cd,Pb,As,Hg,Co,V,Ni in coenzyme Q_(10) were 89.8%-103.5%,and the limits of detection all met the requirements of determination. The elemental impurities in coenzyme Q_(10) material were far below limits. The concentrations of lead in coenzyme Q_(10) capsules made by manufacturers 1-3 were higher than the other. The higher concentration of aluminum in coenzyme Q_(10) capsules made by manufacturers 3 and 14 were supposed come from pharmaceutical excipient talc. Conclusion:The proposed method is accurate,rapid,and sensitive,which can be applied to the determination of elemental impurities in coenzyme Q_(10) material and preparations.
引文
[1]戴惠芳.辅酶Q10立体控制合成的研究[D].上海:复旦大学,2008DAI HF.Studies on The High Stereoselective Synthesis of Coenzyme Q10[D].Shanghai:Fudan Unversity,2008
[2]USP 39-NF-41.VolⅠ[S].2016:268
[3]Guideline for Elemental Impurities ICH Q3D[S].2016
[4]李春盈,张玉英.ICP-MS法测定板蓝根颗粒中重金属及有害元素的含量并分析其来源[J].华西药学杂志,2012,27(2):187LI CY,ZHANG YY.Determination and source apportionment of heavy metals and hazardous elements in Banlangen granules by ICP-MS[J].West Chin J Pharm Sci,2012,27(2):187
[5]杜静,秦民坚,黄林芳,等.ICP-MS测定石斛中微量元素及其安全性评价[Z].世界中联中药专业委员会学术年会暨中药新药研发与中药资源可持续利用国际研讨会,2011DU J,QIN MJ,HUANG LF,et al.Determination of trace elements in Dendorbii caulis by ICP-MS and safety analysis[Z].World Federation of Chinese Medicine Societies(WFCMS)Academic Annual Meeting and International Symposium On the Research and Development of Traditional Chinese Medicine and The Sustainable Use of Traditional Chinese Medicine Resources,2011
[6]牟卫伟,刘艳.ICP-MS测定补钙类保健食品中的多种重金属元素残留[J].中国生化药物杂志,2016,36(5):207MOU WW,LIU Y.Residue determination of various metal elements in calcium health food by ICP-MS[J].Chin J Biochem Pharm,2016,36(5):207
[7]李青,刘思洁,方赤光.食品中铝含量及其危害研究进展[J].食品安全质量检测学报,2016,7(1):14LI Q,LIU SJ,FANG CG.Research progress on the content and harm of aluminum in food[J].Food Safe Qual Detec Technol,2016,7(1):14
[8]欧盟修改有关含铝食品添加剂使用条件和标准[J].国际市场,2012(Z3):50The EU revised the conditions and standards for the use of aluminiumcontaining food additives[J].World Market,2012(Z3):50
[9]USP 39-NF 41.Vol 3[S].2016:5995
[10]中华人民共和国药典2015年版.四部[S].2016:598ChP 2015.VolⅣ[S].2016:598
[2]USP 39-NF-41.VolⅠ[S].2016:268
[3]Guideline for Elemental Impurities ICH Q3D[S].2016
[4]李春盈,张玉英.ICP-MS法测定板蓝根颗粒中重金属及有害元素的含量并分析其来源[J].华西药学杂志,2012,27(2):187LI CY,ZHANG YY.Determination and source apportionment of heavy metals and hazardous elements in Banlangen granules by ICP-MS[J].West Chin J Pharm Sci,2012,27(2):187
[5]杜静,秦民坚,黄林芳,等.ICP-MS测定石斛中微量元素及其安全性评价[Z].世界中联中药专业委员会学术年会暨中药新药研发与中药资源可持续利用国际研讨会,2011DU J,QIN MJ,HUANG LF,et al.Determination of trace elements in Dendorbii caulis by ICP-MS and safety analysis[Z].World Federation of Chinese Medicine Societies(WFCMS)Academic Annual Meeting and International Symposium On the Research and Development of Traditional Chinese Medicine and The Sustainable Use of Traditional Chinese Medicine Resources,2011
[6]牟卫伟,刘艳.ICP-MS测定补钙类保健食品中的多种重金属元素残留[J].中国生化药物杂志,2016,36(5):207MOU WW,LIU Y.Residue determination of various metal elements in calcium health food by ICP-MS[J].Chin J Biochem Pharm,2016,36(5):207
[7]李青,刘思洁,方赤光.食品中铝含量及其危害研究进展[J].食品安全质量检测学报,2016,7(1):14LI Q,LIU SJ,FANG CG.Research progress on the content and harm of aluminum in food[J].Food Safe Qual Detec Technol,2016,7(1):14
[8]欧盟修改有关含铝食品添加剂使用条件和标准[J].国际市场,2012(Z3):50The EU revised the conditions and standards for the use of aluminiumcontaining food additives[J].World Market,2012(Z3):50
[9]USP 39-NF 41.Vol 3[S].2016:5995
[10]中华人民共和国药典2015年版.四部[S].2016:598ChP 2015.VolⅣ[S].2016:598