顶空气相色谱法测定依地酸二钠中甲醛残留量  

Determination of Residual Formaldehyde in EDTA-2Na by Headspace Gas Chromatography

作　　者：海乐 龙海燕 

机构地区：[1]湖南省药品检验研究院,长沙410001

出　　处：《中国药师》2018年第3期530-532,共3页China Pharmacist

摘　　要：目的:建立依地酸二钠(EDTA-2Na)中残留甲醛的测定方法。方法:采用顶空气相色谱法测定。Agilent DB-WAX气相毛细管柱(30 m×0.32 mm,0.5μm),分流进样,分流比为2∶1;载气为N_2,流速为1.0 ml·min^(-1);检测器为FID;进样口温度为230℃,检测器温度为260℃;采用程序升温法:起始温度40℃,保持6 min,再以40℃·min^(-1)速率升温到230℃后,维持10min;进样量为1μl。分别取对照品溶液和供试品溶液,95℃加热平衡25 min,顶空进样,按外标法以峰面积计算含量。结果:甲醛标准溶液在5.10~102.00μg·ml^(-1)浓度范围内与峰面积的线性关系良好(r=0.999 7),平均回收率为84.60%(RSD=3.82%,n=9)。结论:本方法简单、快速、准确,可以用于依地酸二钠中甲醛残留量的测定。Objective： To establish a headspace GC method for the determination of residual formaldehyde in EDTA-2Na. Methods： A headspace GC was used to separate the residual solvents on an Agilent DB-WAX（ 30 m × 0. 32 mm,0. 5 μm） capillary column with an FID detector. The carrier gas was nitrogen at the flow rate of 1. 0 ml·min^（-1）. The temperature of the injector was 230 ℃and that of the FID was 260 ℃. The programmed column temperature was set as follows： maintained at 40 ℃ for 6 min,and then raised to 230 ℃ at the rate of 40 ℃ ·min^（-1） and maintained for 10 min. The injection volume was 1μl with the split ratio of 2∶ 1. The reference solvent and sample were filled into the containers of headspace injector and the containers were in equilibrium at 95 ℃ for 25 min. The amount of residual formaldehyde was calculated by an external standard method. Results： There was a good linear relationship of formaldehyde reference solvent within the concentration range of 5. 10-102. 00 μg·ml^（-1）（ r = 0. 999 7）. The average recovery was84. 60%（ RSD = 3. 82%,n = 9）. Conclusion： The method is simple,rapid and accurate for the determination of residual formaldehyde in EDTA-2Na.

关 键 词：顶空气相色谱 依地酸二钠 甲醛 

分 类 号：R927.11[医药卫生—药学]