ICP-MS法同时测定小牛血去蛋白提取物注射液中14种元素的含量
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篇名: ICP-MS法同时测定小牛血去蛋白提取物注射液中14种元素的含量
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摘要: 目的:建立同时测定小牛血去蛋白提取物注射液中14种元素含量的方法。方法:采用电感耦合等离子体质谱法。射频功率为1 350 W,载气(氩气)流量为1.1 L/min,碰撞气(氦气)流量为4.5 L/min,积分时间为1.5 s,等离子体气流量为18 L/min,采样深度为65 mm,进样蠕动泵转速为24.0 r/min,数据采样模式为跳峰模式,重复次数为3次。结果:镉、铅、砷、汞、钴、钒、镍、铊、银、钼、铜、铬、钡、铝的检测质量浓度线性范围分别为0.05~50 μg/L(r=0.999 7)、0.05~50 μg/L(r=0.999 7)、0.05~50 μg/L(r=0.999 8)、0.05~50 μg/L(r=0.999 5)、0.05~50 μg/L(r=0.999 5)、0.05~50 μg/L(r=0.999 8)、0.05~50 μg/L(r=0.999 6)、0.05~50 μg/L(r=0.999 5)、0.05~50 μg/L(r=0.999 5)、0.05~50 μg/L(r=0.999 8)、0.05~50 μg/L(r=0.999 6)、0.05~50 μg/L(r=0.999 6)、0.05~50 μg/L(r=0.999 7)、0.5~70 μg/L(r=0.999 8);定量限分别为0.003 1、0.008 9、0.016 0、0.025 0、0.002 1、0.006 9、0.038 1、0.002 1、0.005 5、0.002 0、0.023 1、0.005 0、0.002 0、0.324 9 μg/L;检测限分别为0.000 9、0.002 7、0.004 8、0.007 5、0.000 6、0.002 1、0.011 4、0.000 6、0.016 5、0.000 6、0.006 9、0.001 5、0.000 6、0.097 5 μg/L;精密度、稳定性、重复性试验的RSD均小于8%;加样回收率分别为87.4%~94.3%(RSD=2.6%,n=9)、110.3%~118.2%(RSD=1.8%,n=9)、89.8%~99.7%(RSD=3.1%,n=9)、77.7%~84.4%(RSD=2.5%,n=9)、105.6%~113.4%(RSD=2.3%,n=9)、106.7%~116.5%(RSD=2.7%,n=9)、89.1%~104.5%(RSD=4.5%,n=9)、105.6%~118.6%(RSD=3.6%,n=9)、77.8%~88.0%(RSD=4.0%,n=9)、106.7%~116.1%(RSD=2.8%,n=9)、88.5%~97.1%(RSD=3.1%,n=9)、80.5%~88.6%(RSD=2.9%,n=9)、85.2%~99.4%(RSD=4.2%,n=9)、97.6%~109.3%(RSD=3.2%,n=9)。结论:该方法操作简便、准确,精密度、稳定性、重复性均较好,可用于同时测定小牛血去蛋白提取物注射液中14种元素的含量。
ABSTRACT: OBJECTIVE: To establish a method for the content determination of 14 elements in Deproteinized calf blood extractives injection. METHODS: Inductively coupled plasma-mass spectrometry (ICP-MS) was adopted. The radiofrequency power was 1 350 W; flow rate of carrier gas (argon) and collision gas (helium) was 1.1 L/min and 4.5 L/min respectively; integration time was 1.5 s; plasma gas flow rate was 18 L/min; depth of sampling was 65 mm; speed of sampling peristaltic pump was 24.0 r/min; data sampling mode was peak-jump acquisition mode; data collection was repeated for 3 times. RESULTS: The linear ranges of Cd, Pb, As, Co, V, Ni, Tl, Ag, Mo, Cu, Cr, Ba and Al were 0.05-50 μg/L (r=0.999 7), 0.05-50 μg/L (r=0.999 7), 0.05-50 μg/L (r=0.999 8)、0.05-50 μg/L (r=0.999 5), 0.05-50 μg/L (r=0.999 5), 0.05-50 μg/L (r=0.999 8), 0.05-50 μg/L (r=0.999 6), 0.05-50 μg/L (r=0.999 5), 0.05-50 μg/L (r=0.999 5), 0.05-50 μg/L (r=0.999 8), 0.05-50 μg/L (r=0.999 6), 0.05-50 μg/L (r=0.999 6), 0.05-50 μg/L (r=0.999 7) and 0.5-70 μg/L (r=0.999 8), respectively. The limits of quantitation were 0.003 1, 0.008 9, 0.016 0, 0.025 0, 0.002 1, 0.006 9, 0.038 1, 0.002 1, 0.005 5, 0.002 0, 0.023 1, 0.005 0, 0.002 0, 0.324 9 μg/L, separately. The limits of determination were 0.000 9, 0.002 7, 0.004 8, 0.007 5, 0.000 6, 0.002 1, 0.011 4, 0.000 6, 0.016 5, 0.000 6, 0.006 9, 0.001 5, 0.000 6, 0.097 5 μg/L, separately. RSDs of precision, stability and repeatability tests were all less than 8%. The recoveries were 87.4%-94.3%(RSD=2.6%, n=9), 110.3%-118.2%(RSD=1.8%,n=9), 89.8%-99.7%(RSD=3.1%,n=9), 77.7%-84.4%(RSD=2.5%,n=9), 105.6%-113.4%(RSD=2.3%,n=9), 106.7%-116.5%(RSD=2.7%,n=9), 89.1%-104.5%(RSD=4.5%,n=9), 105.6%-118.6%(RSD=3.6%,n=9), 77.8%-88.0%(RSD=4.0%,n=9), 106.7%-116.1%(RSD=2.8%,n=9), 88.5%-97.1%(RSD=3.1%,n=9), 80.5%-88.6%(RSD=2.9%,n=9), 85.2%-99.4%(RSD=4.2%,n=9), 97.6%-109.3%(RSD=3.2%,n=9), respectively. CONCLUSIONS: The method is simple, accurate. The precision, stability and repeatability of this method are also good. It is suitable for simultaneous determination of 14 elements in Deproteinized calf blood extractives injection.
期刊: 2019年第30卷第14期
作者: 邵天舒,周长明,余立,郭雷
AUTHORS: SHAO Tianshu,ZHOU Changming,YU Li,GUO Lei
关键字: 小牛血去蛋白提取物注射液;元素;电感耦合等离子体质谱法;含量测定
KEYWORDS: Deproteinized calf blood extractives injection; Element; Inductively coupled plasma-mass spectrometry; Content determination
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