摘要
目的：建立测定健骨注射液中锂（Li）、铍（Be）、镁（Mg）、铝（A1）、钒（v）、铬（Cr）、锰（Mn）、铁（Fe）、钴（co）、镍（Ni）、铜（Cu）、锌（Zn）、砷（As）、硒（Se）、铷（Rb）、锶（sr）、银（Ag）、镉（Cd）、铯（Cs）、钡（Ba）、汞（Hg）、铅（Pb）、铀（U）23种微量元素含量的方法。方法：采用微波消解．电感耦合等离子体质谱法。射频功率为1550W，采样深度为8mm，冷却温度为2cc，碰撞气为氦气，栽气（氩气）流量为1．03L／min，积分时间为0．5S，等离子气流量为15L／min，分子涡轮泵转速为200L／s，四级杆真空度为1．75x10。Pa，采样锥孔径为1．0mm，截取锥孔径为0．4rain，数据采集重复次数为3次。结果：Li、Be、Mg、Al、V、Cr、Mn、Fe、Co、Ni、Cu、zn、As、Se、Rb、Sr、Ag、Cd、Cs、Ba、Pb、U检测质量浓度线性范围均为0～100ng／ml，Hg为0～2．0ng／ml（r均≥0．9996）；检测限为0．0051．652μg/L；精密度、重复性试验的RsD〈7％；所用仪器测定的准确度良好；加样回收率分别为90．03％～96．11％、88．25％～96．76％、83．54％～92．0l％、85．02％～99．18％、91．87％～94．62％、90．31％～92．28％、89．82％～96．99％、83．45％～89．56％、88．55％～92．39％、92．68％～95．18％、89．04％～93．81％、94．76％～103．11％、96．76％～101．39％、98．36％～105．27％、106．97％～119．89％、97．36％～103．46％、89．11％～90．73％、92．37％～95．62％、95．78％～98．22％、91．59％～97．18％、93．93％～97．12％、96．86％～99．22％、106．14％～110．07％，RSD=0．48％～4．24％，n=6。结论：该方法简便、准确，适用于健骨注射液中23种微量元素的同时测定。
OBJECTIVE： To establish a method for the contents determination of Li, Be, Mg, A1, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Ag, Cd, Cs, Ba, Hg, Pb and U in Jiangu injection. METHODS： Microwave digestion-inductively coupled plasma mass spectrometry （MD-ICPMS） was adopted. RF power was 1 550 W, sampling depth was 8 mm, coolant temperature was 2℃, collision gas was He gas, the flow rate of the carrier gas （argon gas） was 1.03 L/min, integration time was 0.5 s, plasma gas flow rate was 15 L/min ,molecular turbo pumb speed was 200 L/s,quadrupole degree of 1.75 -10 3 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 Li, Be, Mg, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Ag, Cd, Cs, Ba, Pb and U were all in 0-100 ng/ml （r≥0.999 6）, Hg was 0-2.0 ng/ml （r≥0.999 6）; the limit of detection was 0.005-1.652 μg/L; RSDs of precisionand reproducibility tests were lower than 7% ;the accuracy determined by the instrument in the test was good; recoveries were 90.03% -96.11% , 88.25% -96.76% , 83.54% -92.01% , 85.02% -99.18% , 91.87% -94.62% , 90.31% -92.28% , 89.82% -96.99% , 83.45% -89.56%, 88.55%-92.39%, 92.68%-95.18%, 89.04% -93.81%, 94.76% -103.11%, 96.76% -101.39%, 98.36% -105.27%, 106.97% -119.89%, 97.36% -103.46%, 89.11% -90.73%, 92.37% -95.62%, 95.78% -98.22%, 91.59% -97.18%, 93.93% -97.12%, 96.86%-99.22% and 106.14%-110.07 % ,RSD=0.48% -4.24% ,n=6. CONCLUSIONS： The method is simple, accurate, and suitable for the simultaneous determination of 23 trace elements in Jiangu injection.
出处
《中国药房》
CAS
北大核心
2016年第36期5153-5155,共3页
China Pharmacy
关键词
健骨注射液
微波消解.电感耦合等离子体质谱法
微量元素
Jiangu injection
Microwave digestion-inductively coupled plasma mass spectrometry
Trace element
