CN107445242B - 一种在海水条件下同步固定多种抗生素的吸附膜 - Google Patents
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Abstract
本发明属于梯度扩散薄膜技术领域,提供了一种在海水条件下固定多种抗生素的吸附膜。一种在海水条件下同步固定多种抗生素的吸附膜,其包括XDA‑1树脂粉末、琼脂糖粉末及超纯水,其质量比为10:1.5:100;吸附膜直径25mm,厚度0.5mm;所述的在海水条件下同步固定多种抗生素的吸附膜呈橘红色。所述的XDA‑1树脂的比表面积为1279m2g‑1,孔径为30nm。本发明的一种在海水条件下同步固定多种抗生素的吸附膜吸附容量大。本发明所制备的吸附膜比表面积大,对弱疏水性抗生素吸附能力强,较其他类型树脂材料,其在海水中对抗生素的吸附量更大、吸附能力更强。
Description
技术领域
本发明属于梯度扩散薄膜技术领域,涉及一种在海水条件下固定多种抗生素的吸附膜。
背景技术
海水中的微污染物是生态与人体健康的重要风险源,具有环境浓度低、污染状况多元复合、健康风险大的特点。海水中抗生素的污染及生态风险尤其值得关注,其能诱发细菌抗药性,导致抗性基因的出现,这样不但会影响生态平衡,还会给人体健康带来极大威胁。因此,测定海水中抗生素的污染水平对评价其生态风险具有重要意义。
常见的抗生素采样方式为主动采样,采样后移至实验室进行前处理、测样。主动采样人力、资源消耗大,样品运输不便利,前处理流程繁琐。与之相对应的被动采样是近些年研究的热点。被动采样省时、省力,在采样过程中同时完成了过滤、富集等前处理步骤,并能提供污染物的时间加权平均浓度。梯度扩散薄膜技术(Diffusive gradients in thin-films,DGT)作为被动采样的一种,其动力学采样的特点较其他被动采样技术而言更加精准、便捷。
目前DGT已被应用于淡水中痕量金属、有机物的测定及海水中痕量金属的测定,其在海水中对于有机物尤其是抗生素的应用未见报道。文献“Journal of EnvironmentalMonitoring.2012,14(6):1523”中使用XAD-18吸附膜装配到DGT中测定了淡水中抗生素,但该吸附膜在高离子强度下性能降低,不能应用于海水条件。海水基质条件表现为碱性pH(7.9-8.2)、高离子强度(约0.7M),大部分抗生素在该pH条件下发生解离,表现为分子态、离子态共存,由于竞争作用、静电排斥及高离子强度条件下吸附材料内部孔隙改变等因素,常用的DGT吸附层无法在此条件下对抗生素表现良好的吸附性能。
XDA-1大孔吸附树脂是一种高交联度、高比表面积的非极性聚合物吸附剂。其高比表面积和连续的孔结构赋予其对抗生素的优异吸附性能。在制药领域被广泛应用于抗生素的分离与提纯。
发明内容
本发明的目的是提供一种以XDA-1大孔吸附树脂为吸附剂制成的适于检测海水中抗生素等弱疏水性有机污染物的DGT结合相,其能克服海水碱性pH及高离子强度对吸附的不利影响。操作便捷,易于组装到DGT中,适于应用于海水中抗生素的测定。
本发明的技术方案:
一种在海水条件下同步固定多种抗生素的吸附膜,其包括XDA-1树脂粉末和琼脂糖粉末,其质量比为10:1.5;吸附膜直径25mm,厚度0.5mm;所述的在海水条件下同步固定多种抗生素的吸附膜呈橘红色。
所述的XDA-1树脂的比表面积为1279m2g-1,孔径为30nm。
本发明的有益效果:
本发明的一种在海水条件下同步固定多种抗生素的吸附膜具有高比表面积,对弱疏水性抗生素吸附能力强。较其他类型树脂材料,其在海水中对抗生素的吸附量更大、吸附能力更强。
本发明的一种在海水条件下同步固定多种抗生素的吸附膜能克服pH及离子强度对吸附膜吸附抗生素的影响,适宜应用于DGT,用以测定海水中抗生素污染。
本发明的一种在海水条件下同步固定多种抗生素的吸附膜的制备方法和制备过程易于控制,不同批次制得的吸附膜性能稳定并具有较高强度。
附图说明
图1是本发明制备的吸附膜和其他类型树脂吸附膜在模拟海水中的抗生素吸附总量对比情况;
图2是组装有本发明制备的海水条件下同步固定多种抗生素的吸附膜的DGT装置结构示意图;
图3(1)是组装有本发明制备的吸附膜的DGT装置对磺胺甲恶唑的吸附量随放置时间的变化图。
图3(2)是组装有本发明制备的吸附膜的DGT装置对恩诺沙星的吸附量随放置时间的变化图。
图3(3)是组装有本发明制备的吸附膜的DGT装置对氯霉素的吸附量随放置时间的变化图。
图中:1塑料外壳;2吸附膜;3扩散膜;4滤膜。
具体实施方式
为更好理解本发明的内容,下面通过实施例对本发明作进一步说明,但所举之例并不限制本发明的保护范围。
实施例1
制备流程如下:
步骤一,制备XDA-1功能化树脂粉末
(1)将XDA-1大孔树脂烘干,用粉碎机研磨;
(2)将研磨后的树脂粉末两次过筛,留用中间部分;
步骤二,将步骤一筛分出的XDA-1树脂粉末,用甲醇进行活化,后用超纯水淋洗;
步骤三,将步骤二活化淋洗后的树脂和琼脂糖粉末、超纯水按10(质量):1.5(质量):100(体积)混匀得到制胶溶液;
步骤四,将步骤三得到的混合溶液置于磁力搅拌器上加热搅拌至澄清透明,趁热灌注至提前预热(50℃)的内部空间厚度为0.5mm的玻璃模具中平放,约30-40min后冷却至室温。
步骤五,将步骤四得到的冷却后的凝胶膜切割成直径为25mm的圆盘,即得所需吸附膜。
优选地,步骤一中所述的两次过筛尺寸为200目和400目,筛分粒径为38和75微米。
优选地,步骤二中所述的活化、洗涤为依次采用甲醇、超纯水进行,所用的树脂、甲醇、超纯水体积比约为1:8:8。
实施例2
将本发明所制备吸附膜置于不同浓度的10mL抗生素模拟海水溶液中,设置的浓度梯度为10、20、50、100、150、200μg/L,摇床震荡吸附24小时。使用超高效液相色谱串联质谱测定吸附前后溶液中抗生素浓度,用以计算吸附膜对抗生素的吸附比例(%)。由表1可以看出,对于大部分抗生素而言,本发明所制备的吸附膜的吸附比例均高于90%,吸附效果优异,表明其应用于DGT测定海水中抗生素的可行性。
表1本发明所制备吸附膜在不同浓度溶液中对抗生素的吸附比例(%)
实施例3
将含有本发明所制备吸附膜的DGT应用于实际海水中抗生素的测定。将DGT浸没于海水中8小时,取出吸附膜,使用5mL含0.1%甲酸的甲醇洗脱吸附膜两次,之后将洗脱液氮吹至近干,再使用初始流动相复溶,最后使用超高效液相色谱串联质谱进行定量分析。被动采样过程中,同时进行主动采样作为对照。结果显示,被动采样和传统的主动采样方式,测得的抗生素水平具有较好的一致性。
表2含有本发明所制备吸附膜的DGT及主动采样在实际海水中的抗生素测定结果
Claims (1)
1.一种在海水条件下同步固定多种抗生素的吸附膜,其特征在于,所述的吸附膜包括XDA-1树脂粉末和琼脂糖粉末,其质量比为10:1.5;吸附膜的直径25mm,厚度0.5mm;吸附膜呈橘红色;所述的XDA-1树脂的比表面积为1279m2/g,孔径为30nm;
所述的在海水条件下同步固定多种抗生素的吸附膜的制备方法,包括以下步骤:
步骤一,制备XDA-1功能化树脂粉末;
(1)将XDA-1大孔树脂烘干,用粉碎机研磨;
(2)将研磨后的树脂粉末两次过筛,留用中间部分;
所述的两次过筛尺寸为200目和400目,筛分粒径为38和75微米;
步骤二,将步骤一筛分出的XDA-1树脂粉末,用甲醇进行活化,后用超纯水淋洗;
步骤三,将步骤二活化淋洗后的树脂和琼脂糖粉末、超纯水按照质量:质量:体积为10:1.5:100的比例混匀得到制胶溶液;
步骤四,将步骤三得到的混合溶液置于磁力搅拌器上加热搅拌至澄清透明,趁热灌注至提前预热至50℃的内部空间厚度为0.5mm的玻璃模具中平放,30-40min后冷却至室温;
步骤五,将步骤四得到的冷却后的凝胶膜切割成直径为25mm的圆盘,即得所需吸附膜。
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