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

Content Determination of 8 Metal Elements in Propylgaclate and Sodium Chloride Injection by Microwave Digestion-inductively Coupled Plasma Mass Spectrometry

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15L/min,四级杆真空度为3.04×10-4Pa,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。

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 was3.04×10^-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 than12%. 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.