CN101726529A - 一种毛细管电泳拆分2,4,5-滴丙酸对映体的新方法 - Google Patents
一种毛细管电泳拆分2,4,5-滴丙酸对映体的新方法 Download PDFInfo
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Abstract
本发明公开了一种毛细管电泳拆分2,4,5-滴丙酸对映体的新方法,包括以下步骤:(1)将外消旋的2,4,5-滴丙酸、有机改性剂与水溶剂混合制成样品溶液,所述的有机改性剂为甲醇或乙腈;(2)配制十二烷基硫酸钠-磷酸缓冲溶液,调节pH至2~3范围内,然后加入手性选择剂γ-环糊精,并控制γ-环糊精的质量终浓度为3~5%;(3)将样品溶液和含有γ-环糊精的十二烷基硫酸钠-磷酸缓冲溶液放入毛细管电泳仪中,加上反向电压,进行拆分。本发明所述的2,4,5-滴丙酸对映体拆分方法简单、准确,为准确、真实的了解和评价此类物质对映体选择性差异提供技术支撑。
Description
(一)技术领域
本发明涉及一种手性除草剂2,4,5-滴丙酸的对映体拆分方法,属于环境污染物分析技术领域。
(二)背景技术
除草剂又称杀草剂,是一类用来杀死植物的药剂。这些药剂能够选择性地作用于特定目标,使其他对于人类有用的农作物不受伤害,或受的伤害较小。据统计,我国目前除草剂每年使用面积以200万hm2递增,如此大量化学除草剂的使用,一方面,它对我们农业发展作出了非常重要的贡献,但同时也造成了一系列的环境问题,如抗药杂草种群的增加、土壤板结、水体污染等,严重地影响了农业的可持续发展和人类的健康安全。
2,4,5-滴丙酸,中文别名为2-(2,4,5-三氯苯氧基)丙酸,英文名称为2-(2,4,5-trichlorophenoxy)propionic acid,分子式C9H7Cl3O3,分子量269.51,纯品为无色无味结晶,在下列溶剂中的溶解度为:水0.014%、丙酮15.2%、苯0.16%、四氯化碳0.024%、乙醚7.13%、庚烷0.017%、甲醇10.5%。熔点181.6℃。半数致死量(大鼠,经口)650mg/kg。
式1
已有研究表明,同一手性除草剂的各对映体之间虽然有着相同的理化性质,但是它们在生理和毒理方面存在着巨大的差异,因此,从对映体层面考虑这些手性除草剂的药效和环境安全性就显得尤为重要,而手性除草剂2,4,5-滴丙酸的拆分则是研究其对映体环境行为差异和环境安全的必要前提,它将对于准确评价2,4,5-滴丙酸在环境和农产品的残留有着十分重要的意义。
(三)发明内容
本发明要解决的技术问题在于提供一种毛细管电泳结合紫外检测技术拆分2,4,5-滴丙酸的方法,为评价其各对映体的残留特征和环境健康风险提供技术支持。
为解决上述技术问题,本发明采用的技术方案如下:
一种拆分2,4,5-滴丙酸的方法,包括以下步骤:
(1)将外消旋的2,4,5-滴丙酸、有机改性剂与水溶剂混合制成样品溶液,所述的有机改性剂为甲醇或乙腈,所述的样品溶液中2,4,5-滴丙酸的浓度为10-2mg/ml~10-1mg/ml,所述有机改性剂的体积浓度不大于1%;
(2)配制十二烷基硫酸钠-磷酸缓冲溶液,调节pH至2~3范围内,然后加入手性选择剂γ-环糊精(γ-CD),并控制γ-环糊精的质量终浓度为3~5%;以得到的含有γ-CD的十二烷基硫酸钠-磷酸缓冲溶液作为运行用的缓冲溶液;
(3)将步骤(1)制得的样品溶液和步骤(2)制得的含有γ-环糊精的十二烷基硫酸钠-磷酸缓冲溶液放入毛细管电泳仪中,加上反向电压,进行拆分。
本发明步骤(1)中,在配制样品溶液时加入了有机改性剂,以增加样品的溶解性。所述样品溶液中有机改性剂的体积浓度优选为0.5~1%。优选有机改性剂为甲醇。
本发明步骤(2)中,配置H3PO4浓度和十二烷基硫酸钠(SDS)浓度都为30~50mmol/L的缓冲溶液,优选其中H3PO4和SDS的摩尔比为1∶1;更优选缓冲溶液中H3PO4浓度和十二烷基硫酸钠(SDS)浓度均为50mmol/L。本发明可采用碱液如饱和氢氧化钠溶液调节缓冲溶液的pH值,优选调节缓冲溶液的pH至2左右。本发明优选含有γ-CD的十二烷基硫酸钠-磷酸缓冲溶液中γ-环糊精的质量终浓度为4%。本发明运行用的缓冲溶液在配制好后使用一次性注射器经过0.45μm的滤膜过滤。
本发明步骤(3)中,在用毛细管进行拆分之前,通常先后用NaOH溶液、水、十二烷基硫酸钠-磷酸缓冲溶液冲洗毛细管,具体推荐按照如下方法进行冲洗:用0.1mol/L NaOH溶液和水分别冲洗2min,然后运行缓冲溶液冲洗2min,之后进行拆分。本发明可在常规拆分条件下进行拆分,如拆分过程中的反向电压控制在15~25kV,优选20kV;进样采用压力进样0.5psi×3s。
本发明的有益效果是:本发明所述的2,4,5-滴丙酸拆分方法简单、准确,为准确、真实的了解和评价此类物质对映体选择性差异提供技术支撑。
(四)附图说明
图1是本发明实施例1中的2,4,5-滴丙酸对映体的拆分效果图。
(五)具体实施方式
下面以具体实施例对本发明的技术方案做进一步说明,但本发明的保护范围不限于此:
实施例1
(1)样品配制:称取5mg的2,4,5-滴丙酸溶于1ml甲醇中,配置成5mg/ml的母液。随后取10μl加到990μl蒸馏水中,配置1ml成0.05mg/ml的样品溶液。
(2)运行缓冲溶液配制:称取2.884g十二烷基硫酸钠(SDS)溶于50ml水中,配成浓度为200mmol/L的溶液。取0.685ml的H3PO4用蒸馏水定容到50ml,配成浓度约为200mmol/L的溶液。接着各取上述溶液12.5ml定容到50ml,配成H3PO4浓度和SDS浓度都为50mM的缓冲溶液,用饱和NaOH溶液调节pH至2左右。最后,取5ml先前所配pH为2的缓冲溶液,称取195mg γ-CD溶于其中,配制成最终运行用的添加手性选择剂的缓冲溶液。运行用的缓冲溶液在配制好后使用一次性注射器经过0.45μm的滤膜过滤。
(3)仪器:使用仪器为Beckman P/ACE MDQ毛细管电泳仪,PDA检测器,32Karat软件(美国,Beckman公司);熔融石英毛细管柱,60cm×50μm,有效长度为50cm(美国,Beckman公司)。
(4)电泳条件:工作电压,20kV(反向电压);检测波长:214nm;柱温:25℃;压力进样:0.5psi×3s;毛细管使用前用0.1mol/LNaOH溶液和水分别冲洗2min,运行缓冲溶液冲洗2min。随后即可拆分。拆分结果如图1所示,其中左边的峰记为峰一,右边的峰记为峰二。
在步骤(4)的实验条件下,将步骤(1)配制得到的样品溶液连续进样5次,得到与图1相似的结果,考察对映体分离的出峰时间、峰面积、峰高的重现性,实验结果如下:1.出峰时间标准偏差:峰一,2.34%,峰二2.55%;2.峰面积的标准偏差:峰一4.13%,峰二3.92%;3.峰高的标准偏差:峰一6.13%,峰二6.02%。由此可见,本发明所述拆分方法具有良好的重现性。
Claims (8)
1.一种拆分2,4,5-滴丙酸对映体的方法,包括以下步骤:
(1)将外消旋的2,4,5-滴丙酸、有机改性剂与水溶剂混合制成样品溶液,所述的有机改性剂为甲醇或乙腈,所述的样品溶液中2,4,5-滴丙酸的浓度为10-2mg/ml~10-1mg/ml,所述有机改性剂的体积浓度不大于1%;
(2)配制十二烷基硫酸钠-磷酸缓冲溶液,调节pH至2~3范围内,然后加入手性选择剂γ-环糊精,并控制γ-环糊精的质量终浓度为3~5%;
(3)将步骤(1)制得的样品溶液和步骤(2)制得的含有γ-环糊精的十二烷基硫酸钠-磷酸缓冲溶液放入毛细管电泳仪中,加上反向电压,进行拆分。
2.如权利要求1所述的拆分2,4,5-滴丙酸对映体的方法,其特征在于所述样品溶液中有机改性剂的体积浓度为0.5~1%。
3.如权利要求1所述的拆分2,4-滴丙酸对映体的方法,其特征在于所述十二烷基硫酸钠-磷酸缓冲溶液中,十二烷基硫酸钠与磷酸的摩尔比为1∶1,所述十二烷基硫酸钠与磷酸的浓度分别为30~50mmol/L。
4.如权利要求3所述的拆分2,4-滴丙酸对映体的方法,其特征在于所述十二烷基硫酸钠-磷酸缓冲溶液中,所述十二烷基硫酸钠与磷酸的浓度均为50mmol/L。
5.如权利要求1所述的拆分2,4,5-滴丙酸对映体的方法,其特征在于调节十二烷基硫酸钠-磷酸缓冲溶液的pH为2。
6.如权利要求1所述的拆分2,4-滴丙酸对映体的方法,其特征在于控制γ-环糊精的质量终浓度为4%。
7.如权利要求1所述的拆分2,4,5-滴丙酸对映体的方法,其特征在于所述的反向电压控制在15~25kV。
8.如权利要求7所述的拆分2,4,5-滴丙酸对映体的方法,其特征在于所述的反向电压控制在20kV。
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