摘要
建立了测定疫苗中游离甲醛含量的柱前衍生化-高效液相色谱法。采用2,4-二硝基苯肼衍生疫苗中游离甲醛,乙腈︰水(65︰35)为流动相,流速为1.0 m L/min,色谱柱为Waters Atlantis T3柱(4.6 mm×250 mm,5μm),检测波长为365 nm。在此方法下,3个不同甲醛浓度样品回收率为98.28%~105.24%,相对标准偏差(RSD)为2.3%。本方法检测限为0.4 mg/L,定量限为1.6 mg/L。游离甲醛浓度在0.0040~1.1930 mg/m L范围内,与甲醛衍生物峰面积呈良好的线性关系(r2=0.9991)。结果表明,该方法分离度高,专属性强,操作简单且不易受疫苗基质和颜色影响,可用于测定疫苗中游离甲醛含量。
Pre-column derivatization HPLC method was established in order to determine the free formaldehyde content in vaccine with 2,4-dinitrophenylhydrazine( DNPH) as the derivatization reagent. The Waters Atlantis T3( 4. 6 mm × 250 mm,5 μm) was used in the analysis. The mobile phase was a mixture of acetonitrile and water with a ratio of 65 to 35 by volume. The flow rate was 1. 0 m L / min. UV detection was made at the wavelength of 365 nm. The recovery of samples was in a range of 98. 28% ~ 105. 24%,with relative standard deviation( RSD) of 2. 3%. The detection limit was 0. 4 mg / L and the quantitation limit was 1. 6 mg / L. The free formaldehyde content in vaccine showed good liner relationship to the peak area within a content range of 0. 0040 ~1. 1930 mg / m L( r2= 0. 9991). This method is separable,specific,simple and not easy to be affected by vaccine's ground substance and color,and might be used for determination of formaldehyde content in vaccine.
出处
《中国兽药杂志》
北大核心
2016年第8期20-23,共4页
Chinese Journal of Veterinary Drug
关键词
高效液相色谱
柱前衍生化
甲醛
疫苗
HPLC
pre-column derivatization
free formaldehyde
vaccine