摘要
目的探讨氯硝柳胺水样保存方法,建立固相萃取-高效液相色谱法（SPE-HPLC）检测水样中氯硝柳胺含量。方法在实验室模拟现场环境,用鱼塘水配制浓度分别为0.50、1.00 mg/L和2.00 mg/L的氯硝柳胺溶液,避光条件下分别在25、4、-40℃和-40℃（反复冻融）保存,或（和）将水样加入0.2%乙酸和2倍体积的乙腈后,过活化后的固相萃取柱、淋洗并吹干,室温下保存,16 d后洗脱、吹干、复溶,HPLC法测定氯硝柳胺含量。结果氯硝柳胺水样在避光下室温（25℃）和冷藏（4℃）保存条件下含量降低;避光冷冻（-40℃）含量无变化,但反复冻融后含量降低。固相萃取法保存样品16 d未见含量降低。SPE-HPLC测定方法回收率在98.12%~100.06%之间,相对标准偏差（RSD）〈5%。结论氯硝柳胺水样保存条件为避光冷冻且不能反复冻融;固相萃取法不需避光冷冻,可简单而有效地对氯硝柳胺水样进行纯化、富集及保存。
Objective To investigate the preservation condition of niclosamide in water samples and establish a high performance liquid chromatography（HPLC） method by solid-phase extraction（SPE） which is used for determination and preservation of niclosamide in water samples.Methods Under the simulated setting in laboratory,niclosamide was formulated into the solutions of 0.50,1.00 mg/L and 2.00 mg/L with fishpond water.The solutions were preserved at 25,4,-40 ℃ and-40 ℃（repeated freezing and thawing）,respectively,or 0.2% acetic acid and twice volume of acetonitrile were added into the water samples,and then the solutions were passed through the activated column,and stored at room temperature,16 days later,the column was washed,dried and re-dissolved,and niclosamide was determined by using the HPLC method.Results The concentration of niclosamide in water samples decreased at 25 ℃ or 4 ℃,and did not change at-40 ℃,but decreased after repeated freezing and thawing.No decrease of niclosamide was found in water samples for 16 days by using SPE.The recovery rate of HPLC was 98.12%-100.06% and the relative standard deviation（RSD） was less than 5%.Conclusions The preservation of niclosamide in water samples is frozen and protected from light without repeated freezing and thawing.The SPE method does not need to be protected from light and freezing,which can simply and effectively purify,concentrate and store niclosamide in water samples.
出处
《中国血吸虫病防治杂志》
CAS
CSCD
北大核心
2011年第2期133-137,共5页
Chinese Journal of Schistosomiasis Control
基金
国家自然科学基金(81071379)
国家重大科技专项(2008ZX10004-011)
国家科技支撑计划(2009BAI78B06)
