Bagheri Habib, Ghambarian Mahnaz, Salemi Amir, Es-Haghi Ali
Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
J Pharm Biomed Anal. 2009 Oct 15;50(3):287-92. doi: 10.1016/j.jpba.2009.04.039. Epub 2009 May 18.
An immersed single drop microextraction (SDME) method was successfully developed for the trace enrichment of formaldehyde from DTP and DT vaccines and diphtheria-tetanus antigen. The formaldehyde was derivatized by means of the Hantzsch reaction. The dehydropyridine derivative was extracted into a microdrop of chloroform that suspended in a 4 ml sample solution for a preset time. The microdrop was then retracted into the microsyringe and injected directly into a gas chromatography-mass spectrometry (GC-MS) injection port. Effects of different parameters such as the type of solvent, extraction time, stirring rate, and temperature were studied and optimized. The limit of detection was 0.22 ng/l and relative standard deviation (RSD) value was 6.2% (n=5). The regression coefficient was satisfactory (r(2)=0.992) and linear range was obtained from 1 to 500 ng/l.
成功开发了一种浸入式单滴微萃取（SDME）方法，用于从白喉破伤风类毒素（DTP）和白喉破伤风疫苗以及白喉破伤风抗原中痕量富集甲醛。甲醛通过汉茨希反应进行衍生化。将脱氢吡啶衍生物萃取到悬浮于4 ml样品溶液中的一滴氯仿微滴中，并保持预设时间。然后将微滴抽回到微量注射器中，并直接注入气相色谱-质谱联用仪（GC-MS）的进样口中。研究并优化了不同参数的影响，如溶剂类型、萃取时间、搅拌速率和温度。检测限为0.22 ng/l，相对标准偏差（RSD）值为6.2%（n = 5）。回归系数令人满意（r(2)=0.992），线性范围为1至500 ng/l。
