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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 |
| 作者： | 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 |
| 阅读数： | 352 次 |
| 本月下载数： | 8 次 |
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