采用微波消解-电感耦合等离子体质谱(ICP-MS)测定法考察蚓激酶中有害元素的残留量
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摘要
目的:建立测定蚓激酶中铬(Cr)、锰(Mn)、铁(Fe)、钴(Co)、镍(Ni)、铜(Cu)、砷(As)、银(Ag)、镉(Cd)、锑(Sb)、钡(Ba)、汞(Hg)、铊(Tl)、铅(Pb)14个有害元素含量的方法。方法:采用微波消解-电感耦合等离子体质谱法,射频功率为1 530 W,冷却温度为4℃,碰撞气为氦气,载气为氩气,载气流量为1.08 L·min~(-1),积分时间为0.3 s,等离子气流量为15 L·min~(-1),四极杆真空度为3.04×10~(-4) Pa,采样锥孔径为1.0 mm,截取锥孔径为0.4 mm,数据采集重复次数为3次。结果:Mn、 Ni与Cu元素检测线性范围为0～500 ng·mL~(-1),Fe元素检测线性范围为0～10 000 ng·mL~(-1),Hg元素检测线性范围为0～10 ng·mL~(-1),其余各元素检测线性范围均为0～100 ng·mL~(-1),r均≥0.999 0;检测下限为0.004～0.7 ng·mL~(-1);精密度的RSD<2%,重复性的RSD<8%;各元素平均加样回收率为95.4%～109.8%(RSD<4%,n=9)。结论:该方法线性回归良好,灵敏度高,准确性好,适用于蚓激酶原料药中有害元素的检测分析。
Objective:To establish a determination method of Cr,Mn,Fe,Co,Ni,Cu,As,Ag,Cd,Sb,Ba,Hg,Tl and Pb in lumbrokinase.Methods:Microwave digestion-inductively coupled plasma mass spectrometry(MD-ICPMS)was adopted.RF power was 1 530 W,cooling temperature was 4℃,collision gas was He gas,the flow rate of the carrier gas(argon gas)was 1.08 L·min~(-1),integration time was 0.3 s,plasma gas flow rate was 15 L·min~(-1),the vacuum degree of quadrupole was 3.04×10~(-4) Pa,sampling cone aperture was 1.0 mm,interception cone aperture was 0.4 mm,and the data collection was repeated 3 times.Results:The linear ranges of Mn,Ni and Cu were 0-500 ng·m L~(-1)(r ≥0.999 0),the linear range of Fe was 0-10 000 ng·mL~(-1),the linear range of Hg was 0-10 ng·mL~(-1) and the linear ranges of other elements were 0-100 ng·mL~(-1)(r ≥0.999 0).RSDs of precision tests were lower than 2.0% and RSDs of reproducibility tests were lower than 8.0%.Average recoveries were 95.4%-109.8%(RSD<4%,n=9).Conclusion:With good linear relationship,sensitivity and accuracy,the method is suitable for detection of harmful elements in lumbrokinase.
Objective:To establish a determination method of Cr,Mn,Fe,Co,Ni,Cu,As,Ag,Cd,Sb,Ba,Hg,Tl and Pb in lumbrokinase.Methods:Microwave digestion-inductively coupled plasma mass spectrometry(MD-ICPMS)was adopted.RF power was 1 530 W,cooling temperature was 4℃,collision gas was He gas,the flow rate of the carrier gas(argon gas)was 1.08 L·min~(-1),integration time was 0.3 s,plasma gas flow rate was 15 L·min~(-1),the vacuum degree of quadrupole was 3.04×10~(-4) Pa,sampling cone aperture was 1.0 mm,interception cone aperture was 0.4 mm,and the data collection was repeated 3 times.Results:The linear ranges of Mn,Ni and Cu were 0-500 ng·m L~(-1)(r ≥0.999 0),the linear range of Fe was 0-10 000 ng·mL~(-1),the linear range of Hg was 0-10 ng·mL~(-1) and the linear ranges of other elements were 0-100 ng·mL~(-1)(r ≥0.999 0).RSDs of precision tests were lower than 2.0% and RSDs of reproducibility tests were lower than 8.0%.Average recoveries were 95.4%-109.8%(RSD<4%,n=9).Conclusion:With good linear relationship,sensitivity and accuracy,the method is suitable for detection of harmful elements in lumbrokinase.
引文
[1]彭鑫.蚓激酶活性及蛋白成分的研究[D].武汉:湖北中医药大学,2016PENG X.Study on Activity and Protein Ingredients of Lunbrokinase[D].Wuhan:Hubei University of Chinese Medicine,2016
[2]李秦晋,符文卉,魏宝阳,等.蚓激酶的抗菌作用研究[J].湖南农业科学,2015(8):8LI QJ,FU WH,WEI BY,et al.Anti-microbial effects of lumbrokinase[J].Hunan Agric Sci,2015(8):8
[3]徐兴,索绪斌,向兰,等.影响广地龙粗提液蚓激酶活力因素的研究[J].广东药学院学报,2016,32(2):159XU X,SUO XB,XIANG L,et al.Study on the factors on the activity of lumbrokinase in the crude extracts of lumbricus[J].J Guangdong Pharm Univ,2016,32(2):159
[4]闫峻,汤立达.蚓激酶的研究与临床应用[J].中草药,2006,37(2):295YAN J,TANG LD.Study and clinical applicat ion of lumbrokinase[J].Chin Tradit Herb Drugs,2006,37(2):295
[5]龚立科,赵凯,金铨,等.微波消解-电感耦合等离子体质谱法测定稻田土壤中的有害元素[J].中国卫生检验杂志,2017,27(5):618GONG LK,ZHAO K,JIN Q,et al.Determination of heavy metals in paddy soil by microwave digestion-inductively coupled plasma mass spectrometry[J].Chin J Health Lab Technol,2017,27(5):618
[6]陈莉,黄丹,陈盛,等.电感耦合等离子体质谱法测定水溶性原料药中痕量镍[J].理化检验-化学分册,2017,53(5):517CHEN L,HUANG D,CHEN S,et al.ICP-MS determination of trace amount of nickel in water soluble raw pharmaceuticals[J].Phys Test Chem Anal(Part B:Chem Anal),2017,53(5):517
[7]宋更申,周丽,刘浦,等.微波消解-电感耦合等离子体质谱法(ICP-MS)测定蛇床子中16种稀土元素[J].药物分析杂志,2016,36(12):2148SONG GS,ZHOU L,LIU P,et al.Determination of 16 rare earth elements in Cnidii Fructus by ICP-MS[J].Chin J Pharm Anal,2016,36(12):2148
[8]左甜甜,李耀磊,陈沛,等.西洋参、山楂、枸杞子中有害元素及有害元素残留量测定及初步风险评估[J].药物分析杂志,2016,36(11):2016ZUO TT,LI YL,CHEN P,et al.Determination and preliminary risk assessment of heavy metals and harmful elements in American ginseng,the fruit of Chinese wolfberry and hawthorn[J].Chin JPharm Anal,2016,36(11):2016
[9]王梅,郑晖.布洛芬原料药中残留有机溶剂和微量金属杂质的检测研究[J].药物分析杂志,2012,32(7):1209WANG M,ZHENG H.Study on determination of residual solvents and trace metal impurities in ibuprofen[J].Chin J Pharm Anal,2012,32(7):1209
[10]李颖,刘雁鸣,粟贵,等.采用ICP-MS法测定苯甲酸钠中Mn、Co、As、Pb元素的含量[J].中南药学,2015,13(7):752LI Y,LIU YM,SU G,et al.Determination of Mn,Co,As and Pb in sodium benzoate by ICP-MS[J].Cent South Pharm,2015,13(7):752
[11]雷超海,张治军,李沛,等.微波消解-电感耦合等离子体质谱法测定动物类中药中的5种有害元素[J].中国药师,2017,20(8):1482LEI CH,ZHANG ZJ,LI P,et al.Determination of 5 hazardous elements in animal traditional Chinese medicines by ICP-MS[J].China Pharm,2017,20(8):1482
[12]中华人民共和国药典2015年版.一部[S].2015:131ChP 2015.VolⅠ[S].2015:131
[13]WS/T 578.3中国居民膳食营养素参考摄入量[S].2017WS/T 578.3 Chinese Dietary Reference Intakes[S].2017
[2]李秦晋,符文卉,魏宝阳,等.蚓激酶的抗菌作用研究[J].湖南农业科学,2015(8):8LI QJ,FU WH,WEI BY,et al.Anti-microbial effects of lumbrokinase[J].Hunan Agric Sci,2015(8):8
[3]徐兴,索绪斌,向兰,等.影响广地龙粗提液蚓激酶活力因素的研究[J].广东药学院学报,2016,32(2):159XU X,SUO XB,XIANG L,et al.Study on the factors on the activity of lumbrokinase in the crude extracts of lumbricus[J].J Guangdong Pharm Univ,2016,32(2):159
[4]闫峻,汤立达.蚓激酶的研究与临床应用[J].中草药,2006,37(2):295YAN J,TANG LD.Study and clinical applicat ion of lumbrokinase[J].Chin Tradit Herb Drugs,2006,37(2):295
[5]龚立科,赵凯,金铨,等.微波消解-电感耦合等离子体质谱法测定稻田土壤中的有害元素[J].中国卫生检验杂志,2017,27(5):618GONG LK,ZHAO K,JIN Q,et al.Determination of heavy metals in paddy soil by microwave digestion-inductively coupled plasma mass spectrometry[J].Chin J Health Lab Technol,2017,27(5):618
[6]陈莉,黄丹,陈盛,等.电感耦合等离子体质谱法测定水溶性原料药中痕量镍[J].理化检验-化学分册,2017,53(5):517CHEN L,HUANG D,CHEN S,et al.ICP-MS determination of trace amount of nickel in water soluble raw pharmaceuticals[J].Phys Test Chem Anal(Part B:Chem Anal),2017,53(5):517
[7]宋更申,周丽,刘浦,等.微波消解-电感耦合等离子体质谱法(ICP-MS)测定蛇床子中16种稀土元素[J].药物分析杂志,2016,36(12):2148SONG GS,ZHOU L,LIU P,et al.Determination of 16 rare earth elements in Cnidii Fructus by ICP-MS[J].Chin J Pharm Anal,2016,36(12):2148
[8]左甜甜,李耀磊,陈沛,等.西洋参、山楂、枸杞子中有害元素及有害元素残留量测定及初步风险评估[J].药物分析杂志,2016,36(11):2016ZUO TT,LI YL,CHEN P,et al.Determination and preliminary risk assessment of heavy metals and harmful elements in American ginseng,the fruit of Chinese wolfberry and hawthorn[J].Chin JPharm Anal,2016,36(11):2016
[9]王梅,郑晖.布洛芬原料药中残留有机溶剂和微量金属杂质的检测研究[J].药物分析杂志,2012,32(7):1209WANG M,ZHENG H.Study on determination of residual solvents and trace metal impurities in ibuprofen[J].Chin J Pharm Anal,2012,32(7):1209
[10]李颖,刘雁鸣,粟贵,等.采用ICP-MS法测定苯甲酸钠中Mn、Co、As、Pb元素的含量[J].中南药学,2015,13(7):752LI Y,LIU YM,SU G,et al.Determination of Mn,Co,As and Pb in sodium benzoate by ICP-MS[J].Cent South Pharm,2015,13(7):752
[11]雷超海,张治军,李沛,等.微波消解-电感耦合等离子体质谱法测定动物类中药中的5种有害元素[J].中国药师,2017,20(8):1482LEI CH,ZHANG ZJ,LI P,et al.Determination of 5 hazardous elements in animal traditional Chinese medicines by ICP-MS[J].China Pharm,2017,20(8):1482
[12]中华人民共和国药典2015年版.一部[S].2015:131ChP 2015.VolⅠ[S].2015:131
[13]WS/T 578.3中国居民膳食营养素参考摄入量[S].2017WS/T 578.3 Chinese Dietary Reference Intakes[S].2017