CN116571223B - 一种带有高容量高选择性涂层的固相微萃取棒及其制备方法和应用 - Google Patents
一种带有高容量高选择性涂层的固相微萃取棒及其制备方法和应用 Download PDFInfo
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- CN116571223B CN116571223B CN202310539688.XA CN202310539688A CN116571223B CN 116571223 B CN116571223 B CN 116571223B CN 202310539688 A CN202310539688 A CN 202310539688A CN 116571223 B CN116571223 B CN 116571223B
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- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 26
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- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 26
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Abstract
本发明提供了一种带有高容量高选择性涂层的固相微萃取棒及其制备方法和应用,属于农兽药残检测技术领域。包括如下步骤:(1)将聚二甲基硅氧烷与PDMS固化剂混合后加水制成油包水型乳化体系,将油包水型乳化体系倒入模具,插入棒体,进行固化;(2)在聚多巴胺液体培养基中接种塔宾曲霉菌,进行培养,得到聚多巴胺培养菌液;(3)将步骤(1)固化后的棒体插入所述聚多巴胺培养菌液中进行微生物改性;(4)在经微生物改性后的棒体表面涂覆含有模板分子的盐酸多巴胺溶液,在棒体表面形成印迹涂层,印迹结束后,洗去模板分子,得到带有高容量高选择性涂层的固相微萃取棒。该固相微萃取棒具有萃取时间短、吸附体积大、特异性强的优点。
Description
技术领域
本发明涉及农兽药残检测技术领域,尤其涉及一种带有高容量高选择性涂层的固相微萃取棒及其制备方法和应用。
背景技术
食品农残、兽残检测是减少食品中毒概率的有效手段。2022年不合格食品存在的问题中,超三成问题为农兽药残留超标和食品添加剂不规范使用问题,因此,从源头检测来抑制农、兽药残对人体的侵害具有重要意义。
对现场农兽药残的现有分析方法包括液液萃取法、固相萃取等。遗憾的是,尽管这些方法足够敏感,但却需要使用大量有毒有机溶剂、长时间的萃取、较小的吸附体积和繁琐的操作步骤,不能满足现场快速、简便检测的需求。例如,固相萃取法需要以下步骤:(1)固相萃取柱的预处理;(2)将样品倒入活化后的SPE小柱,使样品进入吸附剂;(3)洗尽干扰杂质;(4)洗脱及收集分析物。随着科技的发展,又出现一些新型测定方法,例如固相微萃取法(SPME),有望缩短萃取时间,且使用较少溶剂。但是它本身仍然存在着一些显著的缺点,例如萃取纤维价格昂贵,目标化合物的回收率和精密度较低,且无法分离处理那些结合态的目标物质(特别是与大分子),而且也无法高效彻底分离一些极性差异不明显的物质(如植物色素等)。因此,有必要开发一种灵敏、快速、适合现场检测的农兽药残检测方法,以实现实际的应急检测。
搅拌棒吸附萃取技术(SBSE)因其可以在不含或仅含微量有机溶剂的情况下从水相样品中提取和浓缩痕量分析物而受到人们的广泛关注。其反应原理是通过搅拌棒上的涂层材料对目标分析物提取和富集,然后将搅拌棒浸入含有适量洗脱溶剂的小瓶中,再次搅拌以进行解吸,最后将洗脱溶剂引入合适的仪器进行分析,但这些涂层材料选择性较差,更适用于非极性/弱极性物质,在很多情况下萃取性能然不足,限制了搅拌棒吸附萃取技术的广泛应用。因此,提供一种萃取效率高、特异性高、时间短且使用微升溶剂进行样品吸附的涂层材料非常有必要。
基于此,特提出本发明。
发明内容
本发明提供了一种带有高容量高选择性涂层的固相微萃取棒及其制备方法和应用。以解决现有的样品前处理技术操作浮躁,时间长,且成本高的问题,同时解决目前对搅拌棒吸附萃取涂层的研究存在局限性的问题。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种带有高容量高选择性涂层的固相微萃取棒的制备方法,包括如下步骤:
(1)将聚二甲基硅氧烷与PDMS固化剂混合后加水制成油包水型乳化体系,将油包水型乳化体系倒入模具,插入棒体,进行固化;
(2)在聚多巴胺液体培养基中接种塔宾曲霉菌,进行培养,得到聚多巴胺培养菌液;
(3)将步骤(1)固化后的棒体插入所述聚多巴胺培养菌液中进行微生物改性;
(4)在经微生物改性后的棒体表面涂覆含有模板分子的盐酸多巴胺溶液,在棒体表面形成印迹涂层,印迹结束后,洗去模板分子,得到带有高容量高选择性涂层的固相微萃取棒。
优选的,所述聚二甲基硅氧烷与PDMS固化剂的质量比为8~12:1;所述聚二甲基硅氧烷和PDMS固化剂的总质量与水的质量比为1~2:1;所述固化的温度为100~150℃,所述固化的时间为40~60min。
优选的,所述聚多巴胺液体培养基配方为100~200g去皮马铃薯切块,加水1000ml,将马铃薯煮烂,过滤掉滤渣,取汁液补水至1000ml后加入18~22g琼脂,待琼脂溶解完后,加入18~22g葡萄糖、2~4g磷酸二氢钾、1~2g硫酸镁搅拌均匀;所述塔宾曲霉菌接种到聚多巴胺液体培养基中的接种量为2%~5%(wt);所述培养的温度为25~35℃,时间为4~10天;所述微生物改性的温度为15~35℃,转速为100~300rpm,时间为2~3天。
优选的,所述聚多巴胺液体培养基中还添加了金属离子溶液;所述金属离子溶液为铜离子溶液,所述铜离子溶液的浓度为4~6mmol/L;所述铜离子溶液与聚多巴胺液体培养基的体积比为1:90~110;所述聚多巴胺液体培养基加入金属离子溶液后静置10~14h。
优选的,步骤(4)中所述含有模板分子的盐酸多巴胺溶液按照如下方法配置:将盐酸多巴胺与Tris-HCl缓冲液按照质量体积比80~120mg:40~60mL混合得到盐酸多巴胺溶液,在盐酸多巴胺溶液中加入模板分子溶液和过硫酸铵,得到含有模板分子的盐酸多巴胺溶液;所述Tris-HCl缓冲液的浓度为8~12mmol/L,pH为7.5~8.5。
优选的,所述盐酸多巴胺溶液与模板分子溶液、过硫酸铵的体积质量比为40~60ml:2mL:5mg;所述模板分子溶液的浓度为1~1.2mg/mL;所述模板分子包括绿孔雀石、隐形孔雀石绿、结晶紫和隐形结晶紫中的一种或几种;所述在棒体表面形成印迹涂层的温度为15~25℃,时间为6~24h。
本发明还提供了一种所述的制备方法得到的带有高容量高选择性涂层的固相微萃取棒。
本发明还提供了一种所述的固相微萃取棒上修饰的高容量高选择性涂层。
本发明还提供了一种所述的固相微萃取棒或所述的高容量高选择性涂层在制备检测农兽药残检测产品中的应用。
优选的,所述农兽药残包括绿孔雀石、隐形孔雀石绿、结晶紫或隐形结晶紫。
本发明通过在多孔聚二甲基硅氧烷表面培养塔宾曲霉菌,从而将疏水性聚二甲基硅氧烷改为亲水性物质,同时添加Cu2+离子使塔宾曲霉菌的活性增加,添加铜离子的比不加铜离子的提升105CFU/mL塔宾曲霉菌的活力200%。然后在合成聚多巴胺时利用分子印迹技术将模板分子与盐酸多巴胺聚合,从而赋予其特异性吸附性。如果待测样品中含有模板分子,就会被涂层吸附,在结合便携式质谱仪,根据各组分的离子峰不同,可以判断被提取组分的具体种类。
本发明利用微生物制备带有高容量高选择性涂层的固相微萃取棒的高选择性使得对绿孔雀石(MG)、隐形孔雀石绿(LMG)、结晶紫(CV)、隐形结晶紫(LCV)的萃取时间缩短在50分钟内,更适合实际的现场快速萃取,具有萃取时间短、吸附体积大、特异性强的优点。
本发明的制备工艺简单,无需采用大型设备,反应条件温和,具有成本低,环境友好的优点。
附图说明
图1为实施例1的高容量高选择性涂层的固相微萃取棒的制备和检测示意图。
图2为实施例1制备的高容量高选择性涂层的固相微萃取棒的结构示意图。
具体实施方式
本发明提供了一种带有高容量高选择性涂层的固相微萃取棒的制备方法,包括如下步骤:
(1)将聚二甲基硅氧烷与固化剂混合后加水制成油包水型乳化体系,将油包水型乳化体系倒入模具,插入棒体,进行固化;
(2)在聚多巴胺液体培养基中接种塔宾曲霉菌,进行培养,得到聚多巴胺培养菌液;
(3)将步骤(1)固化后的棒体插入所述聚多巴胺培养菌液中进行微生物改性;
(4)在经微生物改性后的棒体表面涂覆含有模板分子的盐酸多巴胺溶液,在棒体表面形成印迹涂层,印迹结束后,洗去模板分子,得到带有高容量高选择性涂层的固相微萃取棒。
本发明将聚二甲基硅氧烷与固化剂混合后加水制成油包水型乳化体系,将油包水型乳化体系倒入模具,插入棒体,进行固化。
在本发明中,所述聚二甲基硅氧烷与PDMS固化剂的质量比为8~12:1,优选为10:1。
在本发明中,所述聚二甲基硅氧烷与PMDS固化剂总质量与水的质量比为1~2:1,优选为2:1。
在本发明中,所述水优选为去离子水。
在本发明中,所述加水后优选采用高速涡旋乳化,得到稳定的油包水型乳化体系。
在本发明中,所述高速涡旋的转速为500~1000rpm,优选为800rpm;所述高速涡旋的时间为4~6min,优选为5min。
在本发明中,所述模具优选为圆柱形或圆锥形模具,进一步优选为1.5mL离心管。
在本发明中,所述棒体优选为竹棒或聚二甲基硅氧烷-聚多巴胺萃取头,进一步优选为竹棒。
在本发明中,所述棒体的横截面直径优选为2~3mm,进一步优选为2.5mm。
在本发明中,所述固化的温度为100~150℃,优选为120℃;所述固化的时间为40~60min,优选为60min。
本发明在聚多巴胺液体培养基中接种塔宾曲霉菌,进行培养,得到聚多巴胺培养菌液。
在本发明中,聚多巴胺液体培养基配方为100~200g去皮马铃薯切块,加水1000ml,将马铃薯煮烂,过滤掉滤渣,取汁液补水至1000ml后加入18~22g琼脂,待琼脂溶解完后,加入18~22g葡萄糖、2~4g磷酸二氢钾、1~2g硫酸镁搅拌均匀;,优选为150g去皮马铃薯切块,加水1000ml,将马铃薯煮烂,过滤掉滤渣,取汁液补水至1000ml后加入20g琼脂,待琼脂溶解完后,加入20g葡萄糖、3g磷酸二氢钾、1.5g硫酸镁搅拌均匀。
在本发明中,所述聚多巴胺液体培养基分装平板后,以厚度0.003~0.010mm的pu塑料膜覆盖在培养基表面,180℃灭菌20min,室温凝固后备用。
在本发明中,所述塔宾曲霉菌接种到聚多巴胺液体培养基中的接种量为2%~5%(wt),优选为3.5%(wt)。
在本发明中,所述塔宾曲霉菌购自上海晅科生物科技有限公司。
在本发明中,所述培养的温度为25~35℃,优选为30℃;时间为4~10天,优选为7天。
在本发明中,所述聚多巴胺液体培养基中还添加了金属离子溶液。
在本发明中,所述金属离子溶液优选为铜离子溶液,所述铜离子溶液的浓度为优选为4~6mmol/L,进一步优选为5mmol/L。
在本发明中,所述铜离子溶液优选为硫酸铜溶液、氯化铜溶液和硝酸铜溶液的一种或几种。
在本发明中,所述铜离子溶液与聚多巴胺液体培养基的体积比为1:90~110,优选为1:100。
在本发明中,所述聚多巴胺液体培养基加入金属离子溶液后静置10~14h,优选为12h。
本发明将固化后的棒体插入所述聚多巴胺培养菌液中进行微生物改性。
在本发明中,所述微生物改性的温度为15~35℃,优选为30℃;转速为100~300rpm,优选为200rpm;时间为2~3天,优选为3天。
本发明在经微生物改性后的棒体表面涂覆含有模板分子的盐酸多巴胺溶液,在棒体表面形成印迹涂层,印迹结束后,洗去模板分子,得到带有高容量高选择性涂层的固相微萃取棒。
在本发明中,所述含有模板分子的盐酸多巴胺溶液按照如下方法配置:将盐酸多巴胺与Tris-HCl缓冲液按照质量体积比80~120mg:40~60mL混合,优选按照100mg:50mL的质量体积比混合,得到盐酸多巴胺溶液,在盐酸多巴胺溶液中加入模板分子溶液和过硫酸铵,得到含有模板分子的盐酸多巴胺溶液。
在本发明中,所述Tris-HCl缓冲液的浓度为8~12mmol/L,优选为10mmol/L,pH为7.5~8.5,优选为8.0。
在本发明中,所述盐酸多巴胺溶液与模板分子溶液、过硫酸铵的体积质量比为40~60mL:2mL:5mg,优选为50mL:2mL:5mg。
在本发明中,所述模板分子溶液的浓度为1~1.2mg/mL,优选为1mg/mL。
在本发明中,所述模板分子包括绿孔雀石、隐形孔雀石绿、结晶紫和隐形结晶紫中的一种或几种。
在本发明中,所述在棒体表面形成印迹涂层的温度为15~25℃,优选为20℃,时间为6~24h,优选为15h。
在本发明中,所述印迹结束后,优选对棒体进行清洗去除菌落,再作灭菌处理,此时菌落的直径在58~76mm之间,优选在68~73mm之间。
在本发明中,所述灭菌的温度优选为100~150℃,进一步优选为150℃;灭菌的时间优选为10~15min,进一步优选为10min。
在本发明中,所述洗去模板分子的方法为:用J甲醇/乙酸(9:1,v/v)的混合溶液索氏抽提18h,以除去聚合物中的模板分子,将抽提后的固体物质用水和乙醇交替清洗,除去多余的乙酸,60℃下真空干燥。
本发明还提供了一种根据所述的制备方法得到的带有高容量高选择性涂层的固相微萃取棒。
本发明还提供了一种所述的固相微萃取棒上修饰的高容量高选择性涂层。
本发明还提供了一种所述的固相微萃取棒或所述的高容量高选择性涂层在制备检测农兽药残检测产品中的应用。
在本发明中,所述农兽药残包括绿孔雀石、隐形孔雀石绿、结晶紫或隐形结晶紫。
下面结合实施例对本发明提供的技术方案进行详细的说明,但是不能把它们理解为对本发明保护范围的限定。
实施例1
高容量高选择性涂层的固相微萃取棒的制备和检测示意图如图1所示。
将聚二甲基硅氧烷和pdms固化剂以10:1的比例混匀,再按照聚二甲基硅氧烷和pdms固化剂总质量:去离子=2:1的质量比在聚二甲基硅氧烷和pdms固化剂的混合物中加入去离子水,在800rpm下高速涡旋5min,使其乳化形成稳定的油包水型乳化体系。取该乳化体系1.3mL倒入1.5mL离心管中,插入横截面直径为2.5mm的竹棒,在120℃温度下固化60min。
配置5mmol/L的铜离子溶液取1mL加入到100mL的聚多巴胺液体培养基中,混合均匀后静置12h,然后按照3.5%wt的接种量接种塔宾曲霉菌,在30℃培养7天,得到聚多巴胺培养菌液。
将将固化的竹棒插入聚多巴胺培养菌中,置于恒温培养箱,在30℃,200rpm培养3天,取出清洗菌落(菌落直径在58~76mm之间),并在150℃下灭菌10min,得到微生物改性的聚二甲基硅氧烷棒体。
配置含有模板分子的盐酸多巴胺溶液:将盐酸多巴胺与Tris-HCl缓冲液(10mmol/L,pH=8.0)按照质量体积比100mg:50mL混合,然后分别加入模板分子(孔雀石绿、隐形孔雀石绿、结晶紫、隐形结晶紫,浓度均为1mg/mL,添加体均为2mL),5mg过硫酸铵(APS)。混合均匀后涂覆在经微生物改性的聚二甲基硅氧烷棒体的表面,然后在室温(20℃)下搅拌反应10h。之后,将所得到的聚合物进行磁性分离,并用甲醇/乙酸(9:1,v/v)混合溶液索氏提取18h,以除去聚合物中的模板分子。将所得固体物质用水和乙醇交替洗涤,以除去多余的乙酸,最后,磁性分离,60℃下真空干燥,得到带有高容量高选择性涂层的固相微萃取棒,结构示意图,如图2。
实施例2
取新鲜鱼肉的可食用肌肉组织作为样品,测试实施例1制备的固相微萃取棒的性能。
将新鲜鱼肉的可食用肌肉组织经均质机均质后,取0.5g均质机均质后的鱼肉可食用肌肉匀组织浆于50mL离心管中,加入20mL盐酸(0.1mol/L),涡旋混合1min,在室温下超声10分钟进行提取,8000r/min离心5min,取上清液,用NaOH(0.1mol/L)调节样品溶液pH至6.5,再8000r/min离心5min,上清液即为提取液。
取10mL提取液中于容量为10mL的干净玻璃烧杯中,加入0.5%NaCl(w/v),放入磁力搅拌子,将固相微萃取棒悬挂浸入其中,800rpm磁力搅拌35min。取出置于0.2mL乙腈中解吸8min。将解吸后的溶液用便携式质谱仪的电喷雾电离源正离子模式(ESI+)分析,进样口温度为200℃,ESI电压为2kV,鞘气和辅助汽流速为2.5L/min,对四种目标分析物同时检测的时间设置为0.2min。对提取液的测试结果如表1所示。
表1目标分析物监测离子对
分析物 | 监测离子对(m/z) |
MG | 329/313a、329/208 |
LMG | 331/316a、331/239 |
CV | 372/356a、372/251 |
LCV | 374/359a、374/238 |
a定量离子
分别配置1μg/kg、2μg/kg、4μg/kg的MG、LMG、CV、LCV,将同浓度的4中物质混合,得到三种浓度的混合物加标样品(提取液),采用与提取液相同的便携式质谱仪检测条件进行检测,结果表2,三个浓度的加标样品中,MG、LMG、CV和LCV的加标回收率范围分别为84.5-95.3%(RSD=4.6-13.6%),77.8-91.5%(RSD=3.6-15.3%),83.5-97.0%(RSD=4.5-12.9%),82.0-93.5%(RSD=5.2-11.5%)。说明本发明提供的固相微萃取棒对兽药残留检测的准确性高、选择性高。且检测时间低于50分钟。
表2对鱼肉样品提取液的测试结果
由以上实施例可知,本发明利用微生物制备带有高容量高选择性涂层的固相微萃取棒的高选择性使得对绿孔雀石(MG)、隐形孔雀石绿(LMG)、结晶紫(CV)、隐形结晶紫(LCV)的萃取时间缩短在50分钟内,更适合实际的现场快速萃取,具有萃取时间短、吸附体积大、特异性强的优点。同时,本发明的制备工艺简单,无需采用大型设备,反应条件温和,具有成本低,环境友好的优点。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (8)
1.一种带有高容量高选择性涂层的固相微萃取棒的制备方法,其特征在于,包括如下步骤:
(1)将聚二甲基硅氧烷与PDMS固化剂混合后加水制成油包水型乳化体系,将油包水型乳化体系倒入模具,插入棒体,进行固化;
(2)在聚多巴胺液体培养基中接种塔宾曲霉菌,进行培养,得到聚多巴胺培养菌液;
(3)将步骤(1)固化后的棒体插入所述聚多巴胺培养菌液中进行微生物改性;
(4)在经微生物改性后的棒体表面涂覆含有模板分子的盐酸多巴胺溶液,在棒体表面形成印迹涂层,印迹结束后,洗去模板分子,得到带有高容量高选择性涂层的固相微萃取棒;
所述聚多巴胺液体培养基中还添加了金属离子溶液,所述金属离子溶液为铜离子溶液;
步骤(4)中所述含有模板分子的盐酸多巴胺溶液按照如下方法配置:将盐酸多巴胺与Tris-HCl缓冲液按照质量体积比80~120mg:40~60mL混合得到盐酸多巴胺溶液,在盐酸多巴胺溶液中加入模板分子溶液和过硫酸铵,得到含有模板分子的盐酸多巴胺溶液;所述Tris-HCl缓冲液的浓度为8~12mmol/L,pH为7.5~8.5;
所述模板分子包括绿孔雀石、隐形孔雀石绿、结晶紫和隐形结晶紫中的一种或几种。
2.如权利要求1所述的制备方法,其特征在于,所述聚二甲基硅氧烷与PDMS固化剂的质量比为8~12:1;所述聚二甲基硅氧烷和PDMS固化剂的总质量与水的质量比为1~2:1;所述固化的温度为100~150℃,所述固化的时间为40~60min。
3.如权利要求2所述的制备方法,其特征在于,所述聚多巴胺液体培养基配方为:100~200g去皮马铃薯切块,加水1000ml,将马铃薯煮烂,过滤掉滤渣,取汁液补水至1000ml后加入18~22g琼脂,待琼脂溶解完后,加入18~22g葡萄糖、2~4g磷酸二氢钾、1~2g硫酸镁搅拌均匀;
所述塔宾曲霉菌接种到聚多巴胺液体培养基中的接种量为2wt%~5wt%;所述培养的温度为25~35℃,时间为4~10天;所述微生物改性的温度为15~35℃,转速为100~300rpm,时间为2~3天。
4.如权利要求3所述的制备方法,其特征在于,所述铜离子溶液的浓度为4~6mmol/L;所述铜离子溶液与聚多巴胺液体培养基的体积比为1:90~110;所述聚多巴胺液体培养基加入金属离子溶液后静置10~14h。
5.如权利要求1~4任一项所述的制备方法,其特征在于,所述盐酸多巴胺溶液与模板分子溶液、过硫酸铵的体积质量比为40~60ml:2mL:5mg;所述模板分子溶液的浓度为1~1.2mg/mL;所述在棒体表面形成印迹涂层的温度为15~25℃,时间为6~24h。
6.一种根据权利要求1~5任一项所述的制备方法得到的带有高容量高选择性涂层的固相微萃取棒。
7.一种权利要求6所述的固相微萃取棒上修饰的高容量高选择性涂层。
8.一种权利要求6所述的固相微萃取棒或权利要求7所述的高容量高选择性涂层在制备检测农兽药残检测产品中的应用,其特征在于,所述农兽药残包括绿孔雀石、隐形孔雀石绿、结晶紫或隐形结晶紫。
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101590394A (zh) * | 2009-06-18 | 2009-12-02 | 中山大学 | 分子印迹吸附萃取搅拌棒的制备方法及其应用 |
CN103111260A (zh) * | 2013-03-22 | 2013-05-22 | 南京医科大学 | 哑铃状分子印迹搅拌棒的制备方法 |
CN109507126A (zh) * | 2018-12-07 | 2019-03-22 | 集美大学 | 一种水产品中孔雀石绿检测方法 |
CN109839452A (zh) * | 2017-11-29 | 2019-06-04 | 湖南省产商品质量监督检验研究院 | 分子印迹搅拌棒及其制备方法和应用 |
CN112892504A (zh) * | 2021-03-17 | 2021-06-04 | 常新园 | 一种工业污水处理用吸附剂及其制备方法 |
CN114705656A (zh) * | 2022-04-02 | 2022-07-05 | 宁波大学 | 一种基于致毒菌株印迹人工抗体结合噬菌体修饰的长周期光纤光栅及其制备方法和应用 |
CN116083222A (zh) * | 2023-02-09 | 2023-05-09 | 宁波大学 | 一种长周期光纤光栅生物传感器耦合微流控芯片及其制备方法与应用 |
-
2023
- 2023-05-15 CN CN202310539688.XA patent/CN116571223B/zh active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101590394A (zh) * | 2009-06-18 | 2009-12-02 | 中山大学 | 分子印迹吸附萃取搅拌棒的制备方法及其应用 |
CN103111260A (zh) * | 2013-03-22 | 2013-05-22 | 南京医科大学 | 哑铃状分子印迹搅拌棒的制备方法 |
CN109839452A (zh) * | 2017-11-29 | 2019-06-04 | 湖南省产商品质量监督检验研究院 | 分子印迹搅拌棒及其制备方法和应用 |
CN109507126A (zh) * | 2018-12-07 | 2019-03-22 | 集美大学 | 一种水产品中孔雀石绿检测方法 |
CN112892504A (zh) * | 2021-03-17 | 2021-06-04 | 常新园 | 一种工业污水处理用吸附剂及其制备方法 |
CN114705656A (zh) * | 2022-04-02 | 2022-07-05 | 宁波大学 | 一种基于致毒菌株印迹人工抗体结合噬菌体修饰的长周期光纤光栅及其制备方法和应用 |
CN116083222A (zh) * | 2023-02-09 | 2023-05-09 | 宁波大学 | 一种长周期光纤光栅生物传感器耦合微流控芯片及其制备方法与应用 |
Non-Patent Citations (1)
Title |
---|
Preparation, characterization and evaluation of a hybrid polymeric coating with sorbent properties;M. J. Burgos-Tan等;CHEMICAL PAPERS;20161223;第71卷(第7期);1205-1215 * |
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