Determination of Aziridine by HPLC
摘 要
提出了一种测定氮丙啶的高效液相色谱分析方法。将自制氮丙啶单体与福林试剂(1,2-萘醌-4-磺酸钠盐)反应得到衍生物,通过NMR和IR表征验证衍生物结构。衍生物在Agilent ODB C18色谱柱(250 mm×4.6 mm,5 μm)上分离,以乙腈-0.04 mol·L-1磷酸氢二钠混合溶液为流动相进行梯度洗脱,检测波长为258 nm。氮丙啶的线性范围为1.00~20.0 mg·L-1,检出限(3S/N)为0.05 mg·L-1,测定值的相对标准偏差(n=6)小于2%。
Abstract
A HPLC was applied to the determination of aziridine. Self-made aziridine monomer was derivatized with Folin′s reagent (1,2-naphthoquione-4-sulphonic acid) and the structure of the derivate was characterized by NMR and IR. For determination of aziridine, the derivate was seperated on Agilent ODB-C18 (250 mm×4.6 mm, 5 μm) column, using a mixtrure of acetonitrile and 0.04 mol·L-1 sodium phosphate dibasic dodecahydrate solution as mobile phase in gradient elution. The wavelength used in UV-detection was 258 nm. The linearity range for aziridine was in the range of 1.00-20.0 mg·L-1, the detection limit (3S/N) was 0.05 mg·L-1, and RSD′s (n=6) found were less than 2%.
中图分类号 O657.61 DOI 10.11973/lhjy-hx201509021
所属栏目 工作简报
基金项目 浙江省公益性技术应用研究资助项目(2012C23012)
收稿日期 2014/8/22
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联系人作者范红伟(Fanhw@126.com)
备注范红伟(1966-)女,浙江嵊州人,高级工程师,硕士, 主要研究方向为色谱分析。
引用该论文: FAN Hong-wei,WANG Guo-qin,JIANG Jun,TANG Yu-xun. Determination of Aziridine by HPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(9): 1294~1297
范红伟,王国琴,江俊,汤玉训. 高效液相色谱法测定氮丙啶[J]. 理化检验-化学分册, 2015, 51(9): 1294~1297
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参考文献
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【2】MURAV′EVA S I, VINOKUROVA L S. Determination of ethylenimine and monoethanolamine in urine[J]. Gigiena Truda i Professional′nye Zabolevaniya, 1975,11:58-59.
【3】BYKHOVSKAYA M S, MAKEDONSKAYA R N. Determination of ethylenimine in the presence of monoethanolamine and polyethylenimine in the air of industrial establishments[J]. Zhurnal Analiticheskoi Khimii, 1967,22(4):621-623.
【4】PANAGIOTIS G, FRANZ D R. Determination of low levels of aziridine in official EU food simulants by capillary gas chromatography[J]. Lebensm Unters Forsch A, 1997,204:227-230.
【5】EVANS D J, MAYFIELD R J, RUSSELL I M. Rapid estimation of trace amounts of ethylenimine by high-pressure liquid chromatography[J]. Journal of Chromatography, 1975,115(2):391-395.
【6】MAY E M, HUNT D C, SLOGGEM J. A normal-phase high-performance liquid chromatographic assay for aziridine residue in trientine dihydrochloride[J]. Journal of Pharmaceutical and Biomedical Analysis, 1987,5(1):65-70.
【7】ZAPATA J, TEMPRADO J, VIVARACHO L M, et al. Fast and fully automated analytical method for the screening of residues of aziridine and 2-chloroethylamine in pharmaceutical active principles[J]. Journal of Pharmaceutical and Biomedical Analysis, 2011,55:458-465.
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