CN1585897A - 阳离子表面活性剂定量法 - Google Patents
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Abstract
样品溶液中阳离子表面活性剂的定量方法,其特征在于,将样品溶液通过由苯乙烯-二乙烯基苯共聚物颗粒填充的板与用阴离子交换树脂填充的板,然后进行高效液相色谱。利用本发明的方法可以对与无机离子和高浓度AS共存的河流水和湖沼水中ppb级或更低水平的CS进行分离定量。
Description
技术领域
本发明涉及能在环境水等的阴离子表面活性剂和阳离子表面活性剂共存的水溶液中,准确且迅速地对阳离子表面活性剂进行定量的方法及其相关设备。
背景技术
阳离子表面活性剂(CS)作为护发素、治疗剂(treatment)、衣料柔软润饰剂等的主要成分而被广泛应用。但是,由于CS具有杀菌消毒性、难于被微生物降解、其对水生生物的不良影响为人们所忧虑。因此,对环境水中的CS进行定量非常重要,需要建立低浓度CS的快速分析法。
本发明的发明人现利用导电率检测高效液相色谱(HPLC),以建立环境水中CS的高灵敏性分离定量法为目的,对亲水性高分子凝胶柱作为分离柱的HPLC***进行了研究。由所得的结果构建出与现有的利用导电率和间接UV吸光检测的HPLC法相比,测定范围低出一位以上(0.03-0.04μM)的高灵敏的HPLC***。
由于河流中的CS浓度在ppb水平或以下,待进行定量的样品中需要进行CS的浓缩以及无机离子和阴离子表面活性剂(AS)之间的分离。
因此,本发明的目的是提供一种对含有AS和CS的环境水等的水溶液中的仅对CS进行精确定量的方法。
发明内容
因此,本发明的发明人为将样品溶液中的AS和CS分开,安装了用各种树脂填充的板进行各种检测,完全出乎意料地发现用苯乙烯-二乙烯基苯共聚物颗粒填充的板与用阴离子交换树脂填充的板进行组合,样品溶液通过这两个板后,AS被选择性地去除,CS得以浓缩,随后必要时进行固相提取后进行HPLC,可以对低浓度的CS进行正确的定量,由此完成了本发明。
也就是说,本发明提供一种样品溶液中阳离子表面活性剂的定量方法,该方法的特征在于:将样品溶液通过由苯乙烯-二乙烯基苯共聚物颗粒填充的板与用阴离子交换树脂填充的板,然后进行高效液相色谱。
其次,本发明提供一种样品溶液中阳离子表面活性剂的定量方法,该方法的特征在于:将样品溶液通过由苯乙烯-二乙烯基苯共聚物颗粒填充的板与用阴离子交换树脂填充的板,再通过固相提取柱,然后进行高效液相色谱。
再次,本发明还提供一种用于样品溶液中阳离子表面活性剂的定量方法的设备,该设备由用苯乙烯-二乙烯基苯共聚物颗粒填充的板与用阴离子交换树脂填充的板与高效液相色谱设备组成。
本发明还进一步提供一种用于样品溶液中阳离子表面活性剂的定量方法的设备,该设备由用苯乙烯-二乙烯基苯共聚物颗粒填充的板与用阴离子交换树脂填充的板与固相提取柱,以及高效液相色谱设备组成。
附图说明
图1是用于本发明的在线固相提取/HPLC***的示意图。
图2是用河流中的水作为样品,经过SDB-XD(SDB颗粒填充板)和ANION-SR(阴离子交换树脂填充板)的板预处理-在线固相提取-HPLC分离后结果的示意图。
图3用河流中的水作为样品,经过SDB-XD和ANION-SR板预处理-在线固相提取-HPLC对CS进行定量分离中,CTMA(十六烷基三甲基铵离子)和TMSA(三甲基硬脂酰铵离子)的标准添加量实验结果。
图中的符号如下所示。
1:样品溶液 7:洗提液
2:纯水 8:废弃物
3:泵 9:分离柱
4:固相提取柱 10:抑制器
5:注射器 11:检测器
6:泵 12:再生液
具体实施方式
本发明的定量法所用的样品溶液可以是任何含有CS的溶液,更具体地可列举出的有河流水、湖沼水等环境水。在河流水和湖沼水中,除CS以外多数情况下还含有AS、无机离子,对它们进行CS定量此前没有很好的方法。
在本发明中,样品溶液首先通过用苯乙烯-二乙烯基苯共聚物(SDB)颗粒填充的板与用阴离子交换树脂填充的板,经过上述的两板可去除样品溶液中的AS、将CS选择性地回收。在许多种的板中,仅这两种板的组合可去除AS,且CS良好的回收率是完全出乎意料的。所述板中的任何一个都可以用纤维填充颗粒固定,所用的纤维是含氟树脂,优选例如特氟隆(注册商标)等。另外,作为阴离子交换树脂,优选季铵盐型阴离子交换树脂。所述的板可以是由スリ一エム公司获得的商品名为エムポア板SDB-XD、エムポア板ANION-SR。而且所述的板任何一个在先使用均可以。
然后通过上述板后的样品,在必要时需经固相提取柱后,再进行高效液相色谱(HPLC)。经过固相提取可将样品中的CS高度浓缩、由此可使通过HPLC进行CS定量的灵敏性大大提高。固相提取优选使用在线固相提取进行浓缩。
如图1所示,通过泵3将纯水2和样品溶液1供给固相提取柱4后,按一定的循环次数进行在线固相提取。用作固相提取中的固相是填充了亲水高分子的固相,例如可使用高度交联的聚乙烯醇凝胶所填充的固相。所述的聚乙烯醇凝胶可以是例如,Hhodex AsahipakGF-310HP(昭和电工(株式会社))。
将经CS浓缩的样品和通过了上述板的样品进行HPLC。HPLC是由图1中的分离柱9、注射器10和检测器11组成。其中,作为分离柱的亲水性高分子填充柱,例如高度交联的聚乙烯醇凝胶填充的柱,更具体地优选Shodex Asahipak GF-310HP(昭和电工(株式会社))。作为注射器可使用阴离子交换膜,例如DIONEX CMMS-II(日本ダイオネクス(株式会社))。
作为检测器11,可列举出的有:导电率检测器、间接UV吸光检测器、质量分析检测器,特别优选导电率检测器和质量分析检测器。应用质量分析检测时,HPLC之前即使不进行固相提取也可以对很低的浓度进行测定,应用导电率测定时,优选在进行HPLC之前进行固相提取。
应用本发明的方法,以含有超过CS100倍以上的AS的河流或湖沼水为对象进行检测时,可以对低于ppb水平的CS进行定量。
实施例
通过下述的实施例可对本发明进行更具体地说明,但本发明不受这些实施例的任何限制。
实施例1
(1)图1是用作在线固相提取/HPLC***的示意图。4,4-联吡啶/盐酸/乙腈用作洗提液7,Shodex Asahipak GF-310HQ(4.6mmI.D.×150mm,6μm)用作分离柱9。进行固相提取的柱4使用填充了与分离柱相同材质但粒径不同的填充剂的柱(4.6mmI.D.×10mm,9μm),注射器10使用DIONEX CMMS-II(日本ダイオネクス(株式会社)),四丁基铵氢氧化物溶液用作再生液12,样品1可用十六烷基三甲基铵离子(CTMA)、四癸基二甲基苄基铵离子(TDDBA)和三甲基硬脂酰铵离子(TMSA)三种。此外使用エムポア板SDB-XD(SDB颗粒填充板)、CATION-SR(阳离子交换树脂填充板)、ANION-SR(阴离子交换树脂填充板)、SDB-RPS(磺化SDB颗粒填充板)。
(2)首先以50mM浓度的CS用エムポア板对CS的吸收浓缩进行研究。即,在样品溶液通过所述板后,用图1中的在线固相提取/HPLC对CS进行定量。向样品溶液中添加盐酸使溶液达到0.1M,以防止CS吸附到玻璃器皿的壁上。结果对CS的吸收效率的优劣顺序为SDB-RPS>SDB-XD>ANION-SR。但是,向溶液中添加5μM左右的AS则可以观察到每板中的CS回收率均明显下降。在各种检测结果中,将SDB颗粒填充的板SDB-XD和阴离子交换树脂填充的板ANION-SR配套使用,在将AS去除的同时可以得到CS的高回收率(95%以上)。这种高回收率是其他板的组合形式所不能达到的。而且,SDB-XD和ANION-SR以顺序或逆序配套使用所得的结果相同。
(3)根据(2)中的结果,将本发明的方法用于测定实际的河流水。图2是从流经船桥市的海老河采集的河流水的色谱图。由于共存物对CS保存时间变化的影响,重复测定的结果确定了CTMA和TMSA的存在。而且经过质谱分析也确认了CTMA和TMSA的存在。据此,用这些与CS相关的标准添加法进行定量,如图3所示获得了良好的直线关系。根据所得结果,计算出CTMA和TMSA在各河流水中的浓度为1.7nM(0.54ppb)、7.0nM(2.5ppb)。
工业实用性
利用本发明的方法可以对与无机离子和高浓度AS共存的河流水和湖沼水中ppb级或更低水平的CS进行分离定量。
Claims (8)
1、一种对样品溶液中阳离子表面活性剂的定量方法,其特征在于,将样品溶液通过由苯乙烯-二乙烯基苯共聚物颗粒填充的板与用阴离子交换树脂填充的板,然后进行高效液相色谱。
2、如权利要求1所述的定量方法,其特征在于,所述样品是含有阳离子表面活性剂和阴离子表面活性剂的水溶液。
3、如权利要求1或2所述的定量方法,其特征在于,所述高效液相色谱的测定手段是质谱分析。
4、一种样品溶液中阳离子表面活性剂的定量方法,其特征在于,溶液通过由苯乙烯-二乙烯基苯共聚物颗粒填充的板与用阴离子交换树脂填充的板,再通过固相提取柱,然后进行高效液相色谱。
5、如权利要求4所述的定量方法,其特征在于,所述样品是含有阳离子表面活性剂和阴离子表面活性剂的水溶液。
6、如权利要求4或5所述的定量方法,其特征在于:所述高效液相色谱的测定手段是导电率和质谱分析。
7、一种用于检测样品溶液中阳离子表面活性剂的装置,其特征在于,该设备由用苯乙烯-二乙烯基苯共聚物颗粒填充的板、用阴离子交换树脂填充的板以及高效液相色谱设备组成。
8、一种用于检测样品溶液中阳离子表面活性剂的装置,其特征在于,该设备由用苯乙烯-二乙烯基苯共聚物颗粒填充的板、用阴离子交换树脂填充的板、固相提取柱以及高效液相色谱设备组成。
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JP2001356859A JP2003156483A (ja) | 2001-11-22 | 2001-11-22 | 陽イオン界面活性剤の定量法 |
JP356859/2001 | 2001-11-22 |
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US (1) | US20050010002A1 (zh) |
EP (1) | EP1447662A1 (zh) |
JP (1) | JP2003156483A (zh) |
CN (1) | CN1585897A (zh) |
AU (1) | AU2002349681A1 (zh) |
WO (1) | WO2003044518A1 (zh) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102085490A (zh) * | 2010-12-27 | 2011-06-08 | 天津博纳艾杰尔科技有限公司 | 一种固相萃取混合填料及固相萃取柱 |
CN101395476B (zh) * | 2005-12-14 | 2012-10-03 | 电化生研株式会社 | 多重耐药葡萄球菌的免疫色谱检测方法和诊断试剂盒 |
CN104792938A (zh) * | 2015-04-10 | 2015-07-22 | 中国石油大学(华东) | 一种测定co2乳液在渗流过程中表面活性剂浓度分布的装置及方法 |
CN109342638A (zh) * | 2018-11-29 | 2019-02-15 | 浙江树人学院 | 一种利用阳离子交换抑制电导法检测卡内腈、季铵盐及其杂质铵、钾、钙离子含量的方法 |
Families Citing this family (1)
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EP2316035A2 (en) * | 2008-07-16 | 2011-05-04 | Radiometer Medical ApS | Thrombin substrate and assay for determining the level of bioactive thrombin in a sample |
Family Cites Families (4)
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JPH01140061A (ja) * | 1987-11-26 | 1989-06-01 | Shimadzu Corp | 高速液体クロマトグラフィによるエーテル系界面活性剤の分析方法 |
JPH05196606A (ja) * | 1991-09-03 | 1993-08-06 | Kao Corp | 界面活性剤の微量定量分析方法 |
JP3345266B2 (ja) * | 1996-05-28 | 2002-11-18 | 横河電機株式会社 | 陰イオン界面活性剤測定装置 |
JPH1073578A (ja) * | 1996-08-30 | 1998-03-17 | Lion Corp | 界面活性剤を構成する親油基成分の分離方法及び測定方法 |
-
2001
- 2001-11-22 JP JP2001356859A patent/JP2003156483A/ja active Pending
-
2002
- 2002-11-15 AU AU2002349681A patent/AU2002349681A1/en not_active Abandoned
- 2002-11-15 US US10/495,575 patent/US20050010002A1/en not_active Abandoned
- 2002-11-15 EP EP20020781789 patent/EP1447662A1/en not_active Withdrawn
- 2002-11-15 WO PCT/JP2002/011937 patent/WO2003044518A1/ja not_active Application Discontinuation
- 2002-11-15 CN CN02822673.9A patent/CN1585897A/zh active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101395476B (zh) * | 2005-12-14 | 2012-10-03 | 电化生研株式会社 | 多重耐药葡萄球菌的免疫色谱检测方法和诊断试剂盒 |
CN102085490A (zh) * | 2010-12-27 | 2011-06-08 | 天津博纳艾杰尔科技有限公司 | 一种固相萃取混合填料及固相萃取柱 |
CN104792938A (zh) * | 2015-04-10 | 2015-07-22 | 中国石油大学(华东) | 一种测定co2乳液在渗流过程中表面活性剂浓度分布的装置及方法 |
CN104792938B (zh) * | 2015-04-10 | 2016-08-24 | 中国石油大学(华东) | 一种测定co2乳液在渗流过程中表面活性剂浓度分布的装置及方法 |
CN109342638A (zh) * | 2018-11-29 | 2019-02-15 | 浙江树人学院 | 一种利用阳离子交换抑制电导法检测卡内腈、季铵盐及其杂质铵、钾、钙离子含量的方法 |
Also Published As
Publication number | Publication date |
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AU2002349681A1 (en) | 2003-06-10 |
US20050010002A1 (en) | 2005-01-13 |
EP1447662A1 (en) | 2004-08-18 |
WO2003044518A1 (fr) | 2003-05-30 |
JP2003156483A (ja) | 2003-05-30 |
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