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微波消解-电感耦合等离子体质谱法测定棓丙酯氯化钠注射液中8种金属元素的含量
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篇名: 微波消解-电感耦合等离子体质谱法测定棓丙酯氯化钠注射液中8种金属元素的含量
TITLE:
摘要: 目的:建立测定棓丙酯氯化钠注射液中8种金属元素含量的方法。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,积分时间为0.3 s,等离子气流量为15 L/min,四级杆真空度为3.04×10-4 Pa,采样锥孔径为1.0 mm,截取锥孔径为0.4 mm,进样速度为0.3 rps,数据采集重复3次;微波消解功率为1 600 W,升温程序为30 min内由室温升温至160 ℃,保持5 min,再以5 ℃/min的速度升温至190 ℃,保持45 min。结果:镁、铝检测质量浓度线性范围均为1~250 ng/mL, 铬、锰、铁、铜、锌、镉检测质量浓度线性范围均为1~100 ng/mL(r均不小于0.999 0);检测限为0.063 6~1.785 0 ng/mL;精密度、稳定性、重复性试验的RSD均小于4%;加样回收率为89.65%~105.60%(RSD为1.57%~3.98%,n=9);耐用性试验的RSD均小于12%。结论:该方法操作简便、准确,精密度、稳定性、重复性、耐用性好,可用于测定棓丙酯氯化钠注射液中8种金属元素的含量。
ABSTRACT: OBJECTIVE: To establish a method for the content determination of 8 metal elements in Propylgaclate and sodium chloride injection. METHODS: Microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS) was adopted.  Radiofrequency power was 1 530 W; cooling temperature was 4 ℃; collision gas was He gas; carrier gas was argon; flow rate of carrier gas was 1.08 L/min; integration time was 0.3 s; plasma gas flow rate was 15 L/min; 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; the speed of sampling was 0.3 rps; data collection was repeated for 3 times. The microwave digestion power is 1 600 W, and the heating process is heated to 160 ℃ at room temperature for 30 min, and maintained at 5 min, and then heated to 190 ℃ at a temperature of 5 ℃/min and maintained 45 min.  RESULTS: The linear range of Mg and Al were 1-250 ng/mL; the linear range of Cr, Mn, Fe, Cu, Zn, Cd were 1-100 ng/mL(all r≥0.999 0). The limits of detection were 0.063 6-1.785 0 ng/mL. RSDs of precision, stability and reproducibility tests were all lower than 4%. The recoveries were 89.65%-105.60%(RSD were 1.57%-3.98%,n=9). RSDs of durablity were all lower than 12%. CONCLUSIONS: The method is simple, accurate, precise, stable, reproducible and durable. It can be used for content determination of 8 metal elements in Propylgaclate and sodium chloride injection.
期刊: 2018年第29卷第12期
编辑: 钟振华,涂明珠,万星,夏红英,程奇珍
AUTHORS: ZHONG Zhenhua,TU Mingzhu,WAN Xing,XIA Hongying,CHENG Qizhen
关键字: 棓丙酯氯化钠注射液;微波消解-电感耦合等离子体质谱法;金属元素
KEYWORDS: Propylgaclate and sodium chloride injection; Microwave digestion-inductively coupled plasma mass spectrometry; Metal elements
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