ICP-MS法同时测定白石脂药材中27种重金属及微量元素的含量
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摘要
目的:建立同时测定不同产地白石脂药材中27种重金属及微量元素含量的方法。方法:样品经湿法消解后,采用电感耦合等离子体质谱法进行测定。载气为氩气,碰撞气为氦气,等离子体气流速为15.0 L/min,载气流速为1.17 L/min,碰撞气体流量为5.0 mL/min,雾化器为Barbinton,采样深度为8.0 mm,雾化室温度为2℃,等离子体射频功率为1.3 kW,蠕动泵转数为30 r/min;采用全定量分析模式,测点数为3,分析时间为0.1 s,重复3次。采用PASW Statistics 18.0软件进行聚类分析。结果:27种重金属及微量元素检测质量浓度的线性范围为0～200μg/L(r≥0.996 5);定量限为0.003 41～75.485μg/L,检测限为0.001 1～24.350 0μg/L;精密度、稳定性、重复性试验的RSD均小于7%;平均加样回收率为72.3%～129.1%,RSD为0.9%～9.4%(n=6);铝含量为0.01～123 220.20 mg/kg,铝是含量最高的元素,锂、钠、镁、钾、钙、钒、锰、铁、钴、镍、锌、镓、硒、铷、锶、钡和铀是微量元素的主成分,可作为特征元素;26批白石脂样品可聚为4类。结论:该方法操作简便、分析快速、灵敏度高,能提高测定结果的精密度和准确性,适用于白石脂中重金属及微量元素的测定。
OBJECTIVE:To establish a method for simultaneous determination of 27 kinds of heavy metals and trace elements in Halloysitum album from different origins. METHODS:The sample was dissolved by wet digestion. Using inductively coupled plasma mass spectrometry(ICP-MS),carrier gas was argon and collision gas was helium;plasma gas flow rate was 15.0 L/min;flow rate of carrier gas was 1.17 L/min and collision gas flow rate was 5.0 mL/min;atomizer was Barbinton,and sampling depth was 8.0 mm;atomizing chamber temperature was 2 ℃;radio frequency power was 1.3 kW;peristaltic pump revolutions was 30 r/min. In full quantitative analysis model,the number of test points was 3,the analysis time was 0.1 s,the repetition was 3 times,clustering analysis was conducted by using PASW Statistics 18.0 software. RESULTS:The linear range of 27 kinds of heavy metals and trace elements were 0-200 μg/L(r≥0.996 5);the quantitative limit was 0.003 41-75.485 μg/L and the detection limit was0.001 1-24.350 0 μg/L. RSDs of precision,stability and repeatability tests were all less than 7%;average recovery was 72.3%-129.1%(RSD was 0.9%-9.4%,n=6). The content of Al was 0.01-123 220.20 mg/kg,and Al was the element with the highest content. Li,Na,Mg,K,Ca,V,Mn,Fe,Co,Ni,Zn,Ga,Se,Rb,Sr,Ba and U were the principal components of trace elements and could be used as characteristic elements;26 batches of Halloysitum Album samples could be grouped into 4 categories. CONCLUSIONS:The established method is simple,fast and highly sensitive,can improve the precision and accuracy of test results,and it is suitable for the determination of heavy metals and trace elements in Halloysitum album.
OBJECTIVE:To establish a method for simultaneous determination of 27 kinds of heavy metals and trace elements in Halloysitum album from different origins. METHODS:The sample was dissolved by wet digestion. Using inductively coupled plasma mass spectrometry(ICP-MS),carrier gas was argon and collision gas was helium;plasma gas flow rate was 15.0 L/min;flow rate of carrier gas was 1.17 L/min and collision gas flow rate was 5.0 mL/min;atomizer was Barbinton,and sampling depth was 8.0 mm;atomizing chamber temperature was 2 ℃;radio frequency power was 1.3 kW;peristaltic pump revolutions was 30 r/min. In full quantitative analysis model,the number of test points was 3,the analysis time was 0.1 s,the repetition was 3 times,clustering analysis was conducted by using PASW Statistics 18.0 software. RESULTS:The linear range of 27 kinds of heavy metals and trace elements were 0-200 μg/L(r≥0.996 5);the quantitative limit was 0.003 41-75.485 μg/L and the detection limit was0.001 1-24.350 0 μg/L. RSDs of precision,stability and repeatability tests were all less than 7%;average recovery was 72.3%-129.1%(RSD was 0.9%-9.4%,n=6). The content of Al was 0.01-123 220.20 mg/kg,and Al was the element with the highest content. Li,Na,Mg,K,Ca,V,Mn,Fe,Co,Ni,Zn,Ga,Se,Rb,Sr,Ba and U were the principal components of trace elements and could be used as characteristic elements;26 batches of Halloysitum Album samples could be grouped into 4 categories. CONCLUSIONS:The established method is simple,fast and highly sensitive,can improve the precision and accuracy of test results,and it is suitable for the determination of heavy metals and trace elements in Halloysitum album.
引文
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[14]陈蓉,李阳,白静,等.湿法消解电感耦合等离子体质谱法测定冬虫夏草产区土壤铅、砷、铬、镉、铜含量[J].成都中医药大学学报,2018,41(4):3-5、11.
[15]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:87、302.
[16]付娟,张海弢,杨素德,等.基于ICP-MS法分析九味熄风颗粒中25种重金属及微量元素[J].中草药,2015,46(21):3185-3189.
[17]张先彩,张春华,黄晓兰,等.ICP-MS法测定英德红茶中的45种元素[J].食品与机械,2018,34(2):62-66、96.
[18]张昂,王飞,钟亚莉,等.微量乙醇对59种无机元素ICP-MS行为的影响[J].分析试验室,2018,37(3):275-279.
[19]邓建,李浩洋,李蓉,等.ICP-AES和ICP-MS测定稻壳中的14种化学元素[J].食品工业,2017,38(7):301-304.
[20]张源和,何敬愉,马娜,等.ICP-MS法测定刺梨和无籽刺梨果实中有害重金属元素[J].食品工业,2017,38(3):283-286.
[2]甘肃省食品药品监督管理局.甘肃省中药材标准:2009年版[S].兰州:甘肃文化出版社,2009:375-376.
[3]国家中医药管理局《中华本草》编委会.中华本草:二卷[M].上海:上海科学技术出版社,1999:332-336.
[4]萨日娜,王丽霞,陈雯,等.20种风药中7种无机元素含量及其相关性研究[J].中国中医药信息杂志,2018,25(5):90-95.
[5]高慧慧,杨立梅,张超,等.ICP-MS法测定赤石脂煅制前后21种可溶性无机元素[J].中成药,2016,38(6):1346-1350.
[6]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:206-207、523.
[7]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):75-81.
[8]王欣美,吴思霖,杨仁康,等.快速湿法消解-电感耦合等离子体质谱法同时测定紫菜中铅、砷、汞、镉含量[J].中国卫生检验杂志,2018,28(23):2835-2837.
[9]严赟,王娟,罗轶.微波消解-电感耦合等离子体质谱法测定健骨注射液中微量元素的含量[J].中国药房,2016,27(36):5153-5155.
[10]刘永利,苏建,范圣浩,等.ICP-MS法测定血栓通注射剂中14种重金属元素含量[J].中医药导报,2016,22(14):51-53.
[11]陈喆.ICP-MS测定螺旋藻保健品中16种稀土元素的含量[J].海峡药学,2016,28(11):52-55.
[12]高斯祺,刘芳.ICP-MS法测定9种降压类中药材中的微量元素[J].湖南农业科学,2017(4):101-103.
[13]林红强,谭静,王涵,等.ICP-MS法同时测定林下西洋参和园地栽培西洋参中14种微量元素的含量[J].中国药房,2018,19(16):2203-2208.
[14]陈蓉,李阳,白静,等.湿法消解电感耦合等离子体质谱法测定冬虫夏草产区土壤铅、砷、铬、镉、铜含量[J].成都中医药大学学报,2018,41(4):3-5、11.
[15]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:87、302.
[16]付娟,张海弢,杨素德,等.基于ICP-MS法分析九味熄风颗粒中25种重金属及微量元素[J].中草药,2015,46(21):3185-3189.
[17]张先彩,张春华,黄晓兰,等.ICP-MS法测定英德红茶中的45种元素[J].食品与机械,2018,34(2):62-66、96.
[18]张昂,王飞,钟亚莉,等.微量乙醇对59种无机元素ICP-MS行为的影响[J].分析试验室,2018,37(3):275-279.
[19]邓建,李浩洋,李蓉,等.ICP-AES和ICP-MS测定稻壳中的14种化学元素[J].食品工业,2017,38(7):301-304.
[20]张源和,何敬愉,马娜,等.ICP-MS法测定刺梨和无籽刺梨果实中有害重金属元素[J].食品工业,2017,38(3):283-286.