口服液类保健食品中18种重金属元素检测
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摘要
本文旨在建立一种基于微波消解-电感耦合等离子质谱(Inductively coupled plasma mass spectrometry,ICP-MS)测定源于中草药的口服液类保健食品中18种重金属元素(Pb、Cd、As、Hg、Cu、Pt、Pd、Ir、Rh、Ru、Os、Mo、Ni、Cr、V、Mn、Fe、Zn)的方法。采用微波消解法处理口服液样品,以Ge、In、Bi元素作为校正基体效应与信号漂移的内标元素,使用ICP-MS对十批样品中18种重金属进行含量测定。结果显示18种重金属标准曲线线性关系良好,R2≥0.999,各元素的检出限在0.0001～2.743 ng/mL之间,精密度RSD在0.49%～4.29%之间,重复性RSD值在1.2%～15%之间,加样回收率在82.74%～122.7%之间;检测两种口服液中18种重金属元素均未超标。表明该方法操作简便、分析速度快、灵敏度高、准确性好,适用于口服液类保健食品中重金属检测,可为保健食品安全性评价提供依据。
A kind of heavy metal elements(Pb, Cd, As, Hg, Cu, Pt, Pd, Ir, Rh, Ru, Os, Mo, Ni, Cr, V, Mn, Fe, Zn) in oral liquid health foods derived from Chinese herbal medicine based on inductively coupled plasma mass spectrometry(ICP-MS) was established in this work.The oral liquid samples were pre-treated by microwave digestion. The Ge, In and Bi elements were used as the internal standard elements for correcting the matrix effect and signal drift. The contents of 18 heavy metals in ten batches of samples were determined by ICP-MS. Results showed that good linear relations of 18 heavy metal standard curves were found, R2≥0.999, the detection limit of each element was between0.0001～2.743 ng/mL, the precision RSD was between 0.49%～4.29%, and the repetitive RSD value was between 1.2% and 15%, the recovery rate of the sample was between 82.74% and 122.7%. The 18 heavy metal elements in the two oral liquids were not exceeded. Results showed that this method is easy to operate, fast in analysis, high in sensitivity and good in accuracy. It is suitable for the detection of heavy metals in oral liquid health foods, and can provide a basis for health food safety evaluation.
A kind of heavy metal elements(Pb, Cd, As, Hg, Cu, Pt, Pd, Ir, Rh, Ru, Os, Mo, Ni, Cr, V, Mn, Fe, Zn) in oral liquid health foods derived from Chinese herbal medicine based on inductively coupled plasma mass spectrometry(ICP-MS) was established in this work.The oral liquid samples were pre-treated by microwave digestion. The Ge, In and Bi elements were used as the internal standard elements for correcting the matrix effect and signal drift. The contents of 18 heavy metals in ten batches of samples were determined by ICP-MS. Results showed that good linear relations of 18 heavy metal standard curves were found, R2≥0.999, the detection limit of each element was between0.0001～2.743 ng/mL, the precision RSD was between 0.49%～4.29%, and the repetitive RSD value was between 1.2% and 15%, the recovery rate of the sample was between 82.74% and 122.7%. The 18 heavy metal elements in the two oral liquids were not exceeded. Results showed that this method is easy to operate, fast in analysis, high in sensitivity and good in accuracy. It is suitable for the detection of heavy metals in oral liquid health foods, and can provide a basis for health food safety evaluation.
引文
[1]GB 16740-2014,食品安全国家标准保健食品[S]GB 16740-2014,National Food Safety Standards Health Food[S]
[2]彭启志.中药材种植基地土壤及中药材中重金属赋存水平的环境变化分析[J].中国医药科学,2015,4:210-213PENG Qi-zhi.Analysis of environmental change of the occurrent level of heavy metal in planting base soil and Chinese medicinal materials[J].China Medicine and Pharmacy,2015,4:210-213
[3]雷泞菲,彭书明,李凛,等.6种常见中草药中重金属元素铅与镉的测定[J].时珍国医国药,2008,19(3):565-566LEI Ning-fei,PENG Shu-ming,LI Lin,et al.The Determination of the heavy elements Pb,Cd in six traditional chinene[J].Lishizhen Medicine and Materia Medica Research,2008,19(3):565-566
[4]何莎莎.原子吸收光谱法在中药材重金属测定中的应用[J].农家参谋,2018,6:238HE Sha-sha.Application of atomic absorption spectrometry in determination of heavy metals in traditional Chinese medicine[J].The Farmers Consultant,2018,6:238
[5]李江,王江瑞,张潇,等.微波消解-原子吸收分光光度法测定不同产地药用忍冬中重金属[J].药物分析杂志,2015,35(6):1054-1057LI Jiang,WANG Jiang-rui,ZHANG Xiao,et al.Determination of heavy metals in medicinal honevsuckle from different areas by microwave digestion atomic absorption spectroscopy[J].Chinese Journal of Pharmaceutical Analysis,2015,35(6):1054-1057
[6]王志嘉,尤海丹,吴志刚.微波消解-原子荧光光谱法测定中药材中铅、镉、砷、汞、锑的含量[J].沈阳药科大学学报,2008,25(5):388-392WANG Zhi-jia,YOU Hai-dan,WU Zhi-gang.Determination of heavy metals in the traditional chinese medicines by microwave digestion-atomic fluorescence spectrometry[J].Journal of Shenyang Pharmaceutical University,2008,25(5):388-392
[7]赵静,刘勇,张艾华,等.不同产地三七中重金属元素的含量测定及分析[J].中国中药杂志,2014,39(20):4001-4006ZHAO Jing,LIU Yong,ZHANG Ai-hua,et al.Determination and analysis of heavy metals content in Panax notoginseng of different origination[J].China Journal of Chinese Materia Medica,2014,39(20):4001-4006
[8]李春香,王玲玲,荆俊杰,等.微波消解/ICP-AES法同时测定中药中Cd、Hg、Pb含量[J].药物分析杂志,2009,29(3):433-436LI Chun-xiang,WANG Ling-ling,JIN Jun-jie,et al.Simultaneous determination the contents of Cd,Hg and Pb in traditional Chinese medicines by microwave digestion and ICP-AES[J].Chinese Journal of Pharmaceutical Analysis,2009,29(3):433-436
[9]陈桂茜,周玲娜,梅新路,等.ICP-MS法测定抗病毒口服液9种元素含量及其质量评价[J].海峡药学,2016,28(11):56-58CHEN Gui-qian,ZHOU Ling-na,MEI Xin-lu,et al.Determination of nine elements in antiviral oral liquid by ICP-MS and its quality assessment[J].Strait Pharmaceutical Journal,2016,28(11):56-58
[10]Mohd R F L,Abu B N K,Sharifah M.A Comparative study of selected trace element content in malay and Chinese traditional herbal medicine(THM)using an inductively coupled plasma-mass spectrometer(ICP-MS)[J].International Journal of Molecular Sciences,2013,14(2):3078-3093
[11]Patriarca M.The contribution of inductively coupled plasma mass spectrometry to biomedical research[J].Microchemical Journal,1996,54(54):262-271
[12]樊正.微波消解技术在重金属检测中的应用[J].安徽预防医学杂志,2010,16(1):67-69FAN Zheng.Application of microwave digestion technology in heavy metal detection[J].Anhui Journal of Preventive Medicine,2010,16(1):67-69
[13]张江义,王小菊,李国敏.微波消解-电感耦合等离子体质谱法同时测定食品中的主、微量元素[J].分析化学,2014,42(11):1706-1709ZHANG Jiang-yi,WANG Xiao-ju,LI Guo-min.Simultaneous determination of trace elements and major elements in food by ICP-MS using microwave digestion for sample preparation[J].Chinese Journal of Analytical Chemistry,2014,42(11):1706-1709
[14]国家药典委员会.中华人民共和国药典[M].第四部.北京:中国医药科技出版社,2015:43-46,205-207Chinese Pharmacopoeia Commission.Pharmacopoeia of People’s Republic of China[M].Beijing:China Medical Science Press,2015:43-46,205-207
[15]赵铁.血清微量元素组学及其在痛风性关节炎病理研究中的应用[D].上海交通大学,2009ZHAO Tie.Serum trace elements profiling and its application in pathological study of gouty arthritis[D].Shanghai Jiao Tong University,2009
[16]张平,马潇,张明童,等.ICP-MS分析不同产地侧柏叶中18种重金属及微量元素[J].中国实验方剂学杂志,2018,24(7):75-81ZHANG Ping,MA Xiao,ZHANG Ming-tong,et al.Determination and analysis of trace elements and heavy metals content in Platycladi cacumen from different origins by ICP-MS[J].Chinese Journal of Experimental Traditional Medical Formulae,2018,24(7):75-81
[17]中华人民共和国对外贸易经济合作部.药用植物及制剂进出口绿色行业标准[S].北京:中国标准出版社,2001Ministry of Foreign Trade and Economic Cooperation.Import and Export Green Standard of Medicinal Plants and Preparations[S].Beijing:Standards Press of China,2001
[18]美国药典委员会.美国药典[S].36版,2012:151-153The United States Pharmacopieial Convention.U.S.Pharmacopeia/National Formulary[S].USP36,2012:151-153
[19]蔡学建,陈锋,杨玲,等.内标法在ICP-MS中的应用[J].广州化工,2015,43(4):156-157,204CAI Xue-jian,CHEN Feng,YANG Ling,et al.Application of internal standard method in ICP-MS[J].Guangzhou Chemical Industry,2015,43(4):156-157,204
[20]王传之.保健食品中8种有害金属元素的ICP-MS同时定量分析研究[D].福建农林大学,2016WANG Chuang-zhi.Determination of 8 harmful metal elements in health food by ICP-MS[D].Fujian Agriculture and Forestry University,2016
[21]杨晓阳,岳媛,黄红,等.ICP-MS及AAS法测定川明参的无机营养元素[J].中药材,2017,40(12):2790-2796YANG Xiao-yang,YUE Yuan,HUANG Hong,et al.Assay of inorganic nutrient elements in Chuanmingshen violaceum roots by ICP-MS and AAS[J].Journal of Chinese Medicinal Materials,2017,40(12):2790-2796
[22]周利,郝庆秀,王升,等.微波消解ICP-MS法对冬虫夏草不同部位5种重金属元素的分布研究[J].中国中药杂志,2017,42(15):2934-2938ZHOU Li,HAO Qing xiu,WANG Sheng,et al.Study on distribution of five heavy metal elements in different parts of Cordyceps sinensis by microwave digestion ICP-MS[J].China Journal of Chinese Materia Medica,2017,42(15):2934-2938
[23]郭丹,陈娜娜,杨西晓,等.电感耦合等离子质谱法测定常通口服液中重金属镉的含量[J].中药新药与临床药理,2005,3:197-201GUO Dan,CHEN Na-na,YANG Xi-xiao,et al.Determination of heavy metal cadmium in Changtong liquid by inductively coupled plasma mass spectrometry[J].Traditional Chinese Drug Research&Clinical Pharmacology,2005,3:197-201
[24]贾薇.中药材中重金属的分析方法及其吸收富集特征研究[D].广州中医药大学,2009JIA Wei.Study on the analytical method and the absorption and accumulation characteristics of heavy mmetals in Chinese medicinal materials[D].Guangzhou University of Chinese Medicine,2009
[2]彭启志.中药材种植基地土壤及中药材中重金属赋存水平的环境变化分析[J].中国医药科学,2015,4:210-213PENG Qi-zhi.Analysis of environmental change of the occurrent level of heavy metal in planting base soil and Chinese medicinal materials[J].China Medicine and Pharmacy,2015,4:210-213
[3]雷泞菲,彭书明,李凛,等.6种常见中草药中重金属元素铅与镉的测定[J].时珍国医国药,2008,19(3):565-566LEI Ning-fei,PENG Shu-ming,LI Lin,et al.The Determination of the heavy elements Pb,Cd in six traditional chinene[J].Lishizhen Medicine and Materia Medica Research,2008,19(3):565-566
[4]何莎莎.原子吸收光谱法在中药材重金属测定中的应用[J].农家参谋,2018,6:238HE Sha-sha.Application of atomic absorption spectrometry in determination of heavy metals in traditional Chinese medicine[J].The Farmers Consultant,2018,6:238
[5]李江,王江瑞,张潇,等.微波消解-原子吸收分光光度法测定不同产地药用忍冬中重金属[J].药物分析杂志,2015,35(6):1054-1057LI Jiang,WANG Jiang-rui,ZHANG Xiao,et al.Determination of heavy metals in medicinal honevsuckle from different areas by microwave digestion atomic absorption spectroscopy[J].Chinese Journal of Pharmaceutical Analysis,2015,35(6):1054-1057
[6]王志嘉,尤海丹,吴志刚.微波消解-原子荧光光谱法测定中药材中铅、镉、砷、汞、锑的含量[J].沈阳药科大学学报,2008,25(5):388-392WANG Zhi-jia,YOU Hai-dan,WU Zhi-gang.Determination of heavy metals in the traditional chinese medicines by microwave digestion-atomic fluorescence spectrometry[J].Journal of Shenyang Pharmaceutical University,2008,25(5):388-392
[7]赵静,刘勇,张艾华,等.不同产地三七中重金属元素的含量测定及分析[J].中国中药杂志,2014,39(20):4001-4006ZHAO Jing,LIU Yong,ZHANG Ai-hua,et al.Determination and analysis of heavy metals content in Panax notoginseng of different origination[J].China Journal of Chinese Materia Medica,2014,39(20):4001-4006
[8]李春香,王玲玲,荆俊杰,等.微波消解/ICP-AES法同时测定中药中Cd、Hg、Pb含量[J].药物分析杂志,2009,29(3):433-436LI Chun-xiang,WANG Ling-ling,JIN Jun-jie,et al.Simultaneous determination the contents of Cd,Hg and Pb in traditional Chinese medicines by microwave digestion and ICP-AES[J].Chinese Journal of Pharmaceutical Analysis,2009,29(3):433-436
[9]陈桂茜,周玲娜,梅新路,等.ICP-MS法测定抗病毒口服液9种元素含量及其质量评价[J].海峡药学,2016,28(11):56-58CHEN Gui-qian,ZHOU Ling-na,MEI Xin-lu,et al.Determination of nine elements in antiviral oral liquid by ICP-MS and its quality assessment[J].Strait Pharmaceutical Journal,2016,28(11):56-58
[10]Mohd R F L,Abu B N K,Sharifah M.A Comparative study of selected trace element content in malay and Chinese traditional herbal medicine(THM)using an inductively coupled plasma-mass spectrometer(ICP-MS)[J].International Journal of Molecular Sciences,2013,14(2):3078-3093
[11]Patriarca M.The contribution of inductively coupled plasma mass spectrometry to biomedical research[J].Microchemical Journal,1996,54(54):262-271
[12]樊正.微波消解技术在重金属检测中的应用[J].安徽预防医学杂志,2010,16(1):67-69FAN Zheng.Application of microwave digestion technology in heavy metal detection[J].Anhui Journal of Preventive Medicine,2010,16(1):67-69
[13]张江义,王小菊,李国敏.微波消解-电感耦合等离子体质谱法同时测定食品中的主、微量元素[J].分析化学,2014,42(11):1706-1709ZHANG Jiang-yi,WANG Xiao-ju,LI Guo-min.Simultaneous determination of trace elements and major elements in food by ICP-MS using microwave digestion for sample preparation[J].Chinese Journal of Analytical Chemistry,2014,42(11):1706-1709
[14]国家药典委员会.中华人民共和国药典[M].第四部.北京:中国医药科技出版社,2015:43-46,205-207Chinese Pharmacopoeia Commission.Pharmacopoeia of People’s Republic of China[M].Beijing:China Medical Science Press,2015:43-46,205-207
[15]赵铁.血清微量元素组学及其在痛风性关节炎病理研究中的应用[D].上海交通大学,2009ZHAO Tie.Serum trace elements profiling and its application in pathological study of gouty arthritis[D].Shanghai Jiao Tong University,2009
[16]张平,马潇,张明童,等.ICP-MS分析不同产地侧柏叶中18种重金属及微量元素[J].中国实验方剂学杂志,2018,24(7):75-81ZHANG Ping,MA Xiao,ZHANG Ming-tong,et al.Determination and analysis of trace elements and heavy metals content in Platycladi cacumen from different origins by ICP-MS[J].Chinese Journal of Experimental Traditional Medical Formulae,2018,24(7):75-81
[17]中华人民共和国对外贸易经济合作部.药用植物及制剂进出口绿色行业标准[S].北京:中国标准出版社,2001Ministry of Foreign Trade and Economic Cooperation.Import and Export Green Standard of Medicinal Plants and Preparations[S].Beijing:Standards Press of China,2001
[18]美国药典委员会.美国药典[S].36版,2012:151-153The United States Pharmacopieial Convention.U.S.Pharmacopeia/National Formulary[S].USP36,2012:151-153
[19]蔡学建,陈锋,杨玲,等.内标法在ICP-MS中的应用[J].广州化工,2015,43(4):156-157,204CAI Xue-jian,CHEN Feng,YANG Ling,et al.Application of internal standard method in ICP-MS[J].Guangzhou Chemical Industry,2015,43(4):156-157,204
[20]王传之.保健食品中8种有害金属元素的ICP-MS同时定量分析研究[D].福建农林大学,2016WANG Chuang-zhi.Determination of 8 harmful metal elements in health food by ICP-MS[D].Fujian Agriculture and Forestry University,2016
[21]杨晓阳,岳媛,黄红,等.ICP-MS及AAS法测定川明参的无机营养元素[J].中药材,2017,40(12):2790-2796YANG Xiao-yang,YUE Yuan,HUANG Hong,et al.Assay of inorganic nutrient elements in Chuanmingshen violaceum roots by ICP-MS and AAS[J].Journal of Chinese Medicinal Materials,2017,40(12):2790-2796
[22]周利,郝庆秀,王升,等.微波消解ICP-MS法对冬虫夏草不同部位5种重金属元素的分布研究[J].中国中药杂志,2017,42(15):2934-2938ZHOU Li,HAO Qing xiu,WANG Sheng,et al.Study on distribution of five heavy metal elements in different parts of Cordyceps sinensis by microwave digestion ICP-MS[J].China Journal of Chinese Materia Medica,2017,42(15):2934-2938
[23]郭丹,陈娜娜,杨西晓,等.电感耦合等离子质谱法测定常通口服液中重金属镉的含量[J].中药新药与临床药理,2005,3:197-201GUO Dan,CHEN Na-na,YANG Xi-xiao,et al.Determination of heavy metal cadmium in Changtong liquid by inductively coupled plasma mass spectrometry[J].Traditional Chinese Drug Research&Clinical Pharmacology,2005,3:197-201
[24]贾薇.中药材中重金属的分析方法及其吸收富集特征研究[D].广州中医药大学,2009JIA Wei.Study on the analytical method and the absorption and accumulation characteristics of heavy mmetals in Chinese medicinal materials[D].Guangzhou University of Chinese Medicine,2009