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.
ABSTRACT
Objective: To establish a method for the determination of eucalyptol, camphor and menthol in compound menthol camphor eucalyptus oil solution by GC.Methods: An HP-INNOWAX 19091N-216 capillary column(60 m× 0.32 mm , 0.50 μm)was used.The carrier gas was nitrogen with the flow rate of 30 ml·min-1 , the gas was hydrogen with the flow rate of 40 ml·min-1 and the oxidant gas was air with the flow rate of 400 ml· min-1.The detector was FID and the inlet temperature was 250℃.The temperature program was as follows: the initial column temperature was 50℃, and then risen to 160℃ with a rate of 10℃·min-1 and kept for 5 min, and finally risen to 220℃ with a rate of 20℃·min-1 and kept for 3 min.The split ratio was 15∶1 and the injection volume was 1 μl.Results: The linear range of eucalyptol, camphor and menthol was 0.031 9-2.550 0 mg·ml-1 (r=1.000 0), 0.041 3-3.305 0 mg·ml-1 (r=1.000 0) and 0.053 7-4.294 0 mg·ml-1 (r=1.000 0), respectively.The average recovery was 98.24% (RSD=0.3% , n =9), 98.97% (RSD=0.4% , n =9) and 98.98% (RSD=0.5% , n =9), respectively.Conclusion: The method is sensitive and accurate with good stability, which can be used to determine the contents of eucalyptol, camphor and menthol in compound menthol camphor eucalyptus oil solution.