KR20110034117A - A sample preparation method for the analysis of triclosan, chlorophenols and acidic pharmaceuticals in water - Google Patents

A sample preparation method for the analysis of triclosan, chlorophenols and acidic pharmaceuticals in water Download PDF

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KR20110034117A
KR20110034117A KR1020090091497A KR20090091497A KR20110034117A KR 20110034117 A KR20110034117 A KR 20110034117A KR 1020090091497 A KR1020090091497 A KR 1020090091497A KR 20090091497 A KR20090091497 A KR 20090091497A KR 20110034117 A KR20110034117 A KR 20110034117A
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water
triclosan
chlorophenols
acidic
liquid chromatography
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김달호
한정호
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한국표준과학연구원
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Abstract

PURPOSE: A method for simultaneously analyzing triclosan, chlorophenols, and acidic pharmaceuticals contained in water is provided to simply implement an analyzing process without a derivatization process. CONSTITUTION: A method for simultaneously analyzing triclosan, chlorophenols, and acidic pharmaceuticals contained in water includes the following: Triclosan, chlorophenols, and acidic pharmaceuticals contained in water are absorbed in carbowax/templated resin fiber. The carbowax/templated resin fiber is in contact with the same solvent as a mobile phase for liquid chromatography. The absorbed extract is desorbed. The desorbed solution is analyzed using liquid chromatography.

Description

물에 함유된 트리클로산, 클로로페놀류, 산성 의약품류의 간단한 동시 분석방법{A sample preparation method for the analysis of triclosan, chlorophenols and acidic pharmaceuticals in water}A sample preparation method for the analysis of triclosan, chlorophenols and acidic pharmaceuticals in water}

본 발명은 특정한 고체상 섬유(carbowax/templated resine, 50 ㎛, CW/TPR)를 이용하여 물에 함유된 휘발성 및 반휘발성 유기 환경 오염물질을 분리, 분석하기 위해 시료를 농축하는 전처리 방법과, 농축된 성분을 액체크래마토그래피에 주입하고 UV 검출기를 이용하여 분석하는 분석 방법에 관한 기술이다.The present invention relates to a pretreatment method for concentrating a sample to isolate and analyze volatile and semivolatile organic environmental contaminants in water using specific solid-phase fibers (carbowax / templated resine, 50 μm, CW / TPR), and It is a technique related to an analytical method in which the component is injected into liquid chromatography and analyzed using a UV detector.

기존의 전처리 방법은 고체상 추출법(solid phase extraction)을 사용하여 여러 단계에 걸쳐 많은 양의 유해한 유기용매를 이용한 전처리를 하여 액체 또는 기체 크래마토그래피로 분리, 분석을 하였다. 고체상 추출법을 이용하여 전처리하는 경우 그 과정이 복잡하고 다량의 시료가 필요하며, 시간이 많이 들고 환경오염 및 건강에 유해한 다량의 유기 용매를 사용하여 경제적으로나 효율적으로 어려움이 있는 기술이었다. 또한 고체상 미량 추출법을 가스 크래마토그래피와 함께 사용 시 분석대상물질들의 극성을 줄이고 휘발성이 있도록 유도체화 하는 과정이 필요하여 방법적으로 시료의 전처리 절차가 복잡하다. Conventional pretreatment methods use solid phase extraction to separate and analyze by liquid or gas chromatography by pretreatment using a large amount of harmful organic solvents in several stages. In case of pretreatment using solid phase extraction method, the process is complicated and a large amount of samples are required, and it is a technology that is economically and efficiently difficult by using a large amount of organic solvent which is time-consuming and harmful to environmental pollution and health. In addition, when the solid phase trace extraction method is used together with gas chromatography, it is necessary to derivatize the analytes to reduce the polarity and volatility of the analyte, and thus, the method of pretreatment of the sample is complicated.

본 발명은 고체상 섬유(carbowax/templated resine, 50 ㎛, CW/TPR)와 액체크래마토그래피를 이용하여 물에 함유된 트리클로산, 크로로페놀, 산성 의약품류를 동시에 신속하고 간편하게 분석할 수 있는 방법을 개발하고자 한다. The present invention is a method that can simultaneously and quickly analyze triclosan, chlorophenol, acidic medicines contained in water using solid phase fibers (carbowax / templated resine, 50 ㎛, CW / TPR) and liquid chromatography We want to develop

구체적으로 본 발명은 물 속에 함유된 트리클로산, 크로로페놀, 산성 의약품류를 유도체화 하는 과정 없이 동시에 분석할 수 있으며, 2 ~ 20ngL-1인 극미량까지 분석할 수 있는 새로운 분석방법을 제공하고자 한다.Specifically, the present invention can be analyzed at the same time without the process of derivatizing triclosan, chlorophenol, acidic medicines contained in water, and to provide a new analysis method that can be analyzed up to a trace amount of 2 ~ 20ngL -1 .

본 발명은 물에 함유된 트리클로산(triclosan), 클로로페놀류, 산성 의약품류를 동시에 분석하는 방법에 관한 것이다. The present invention relates to a method for simultaneously analyzing triclosan, chlorophenols and acidic medicines contained in water.

보다 구체적으로 More specifically

a) 물에 함유된 트리클로산, 클로로페놀류, 산성 의약품류를 CW/TPR(carbowax/templated resine) 섬유로 흡착하는 단계;a) adsorbing triclosan, chlorophenols and acidic medicines contained in water with carbowax / templated resine (CW / TPR) fibers;

b) 상기 CW/TPR 섬유를 액체 크로마토그래피용 이동상과 동일한 용매에 접촉하여 흡착된 추출물을 탈착하는 단계; 및b) contacting the CW / TPR fibers with the same solvent as the mobile phase for liquid chromatography to desorb the adsorbed extract; And

c) 상기 탈착된 용액을 액체크로마토그래피를 이용하여 분석하는 단계;c) analyzing the desorbed solution using liquid chromatography;

를 포함한다.It includes.

상기 a)단계에서 물의 온도는 23 ~ 25℃, pH 범위는 2 ~ 4이며, 추출시간은 10 ~ 60분인 것이 바람직하다.The temperature of the water in step a) is 23 ~ 25 ℃, pH range is 2 to 4, the extraction time is preferably 10 to 60 minutes.

또한, 상기 이동상은 아세토나이트릴 : 10mM 아세트산 수용액이 60 ~ 80 : 20 ~ 40 중량비로 혼합된 것을 사용한다. 상기 액체 크로마토그래피의 고정상은 실리카를 사용하는 것이 바람직하다. In addition, the mobile phase uses a mixture of acetonitrile: 10mM acetic acid aqueous solution in a weight ratio of 60 ~ 80: 20 ~ 40. As the stationary phase of the liquid chromatography, silica is preferably used.

이하 본 발명을 보다 구체적으로 설명한다.Hereinafter, the present invention will be described in more detail.

본 발명은 고체상 섬유를 이용하여 흡착하는 단계와, 흡착된 추출물을 탈착하는 단계로 이루어지며, 흡착하는 단계에 대해 구체적으로 설명하면 고체상 섬유(CW/TPR)를 물에 직접 노출시켜 교반용 막대자석과 교반기를 이용하여 물을 교반해 주면서, 물 중 분석물질 농도에 따라 10~60분간 트리클로산 및 크로로페놀, 산성 약품류를 흡착시킨다. 이후 탈착하는 단계는 고체상 미량 추출법용 인터페이스를 사용하여 미량의 탈착용매에 4 ~ 6분간 노출시켜 탈착시킨 후, 트리클로산, 클로로페놀 및 산성 의약품류를 액체크래마토그래피로 분리, 분석한다.The present invention comprises a step of adsorbing using a solid fiber and a step of desorption of the adsorbed extract, and the specific step of the adsorbing step is to expose the solid fiber (CW / TPR) directly to water to stir the bar magnet While stirring the water using a stirrer and adsorbing triclosan, chlorophenol and acidic chemicals for 10 to 60 minutes depending on the analyte concentration in the water. Thereafter, the step of desorption is performed by exposing to a small amount of desorption solvent for 4 to 6 minutes using an interface for a solid phase trace extraction method, and then separating and analyzing triclosan, chlorophenol and acidic medicines by liquid chromatography.

본 발명에 따른 분석방법에 의하면 트리클로산, 클로로페놀류 및 산성의약품류를 동시에 각각 2 ~ 20ngL-1인 매우 극미량까지 분석할 수 있다.According to the analytical method according to the present invention, triclosan, chlorophenols and acidic pharmaceuticals can be analyzed up to very trace amounts of 2 to 20ngL −1 , respectively.

상기 a) 단계에서 미량 고체상 추출 시 시료인 물의 온도는 23 ~ 25℃, pH 범위는 2 ~ 4, 고체상 추출의 최적시간은 10 ~ 60분이다. 상기 조건에서 트리클로산, 클로로페놀류 및 산성의약품류를 안정적으로 추출할 수 있으며, 성분이 변질되거나 분해되지 않고 안정적으로 분석을 할 수 있다.When the trace solid phase extraction in step a) the temperature of the water sample is 23 ~ 25 ℃, pH range is 2 ~ 4, the optimum time of the solid phase extraction is 10 ~ 60 minutes. Under the above conditions, triclosan, chlorophenols and acidic pharmaceuticals can be stably extracted, and the components can be stably analyzed without alteration or degradation.

상기 a) 단계에서 추출 시 교반을 하는 것이 바람직하며, 교반속도는 800 ~ 1200rpm이 적당하다. It is preferable to stir at the time of extraction in step a), and the stirring speed is suitably 800 to 1200 rpm.

상기 추출 과정을 거친 고체상 섬유는 전용 홀더를 이용하여 고체상 미량 추출법용 인터페이스에 장착한 후, 액체 크로마토그래피용 이동상과 동일한 용매를 흘려주며 탈착시킨다. 상기 이동상은 아세토나이트릴 : 10mM 아세트산 수용액이 60 ~ 80 : 20 ~ 40 중량비로 혼합된 것을 사용한다. 보다 바람직하게는 70 : 30 중량비로 혼합하여 사용한다. 탈착시간은 4 ~ 6분, 0.5 ~ 3mL/min의 유속으로 흘려주며 탈착한다. 상기 이동상을 이용하는 경우 트리클로산, 클로로페놀류 및 산성의약품류의 분리효능이 우수하며, 동시 분석이 가능하고, 정량한계가 2 ~ 20ngL-1인 극미량도 분석을 할 수 있다.The solid fibers subjected to the extraction process are attached to the interface for solid phase micro extraction using a dedicated holder, and then desorbed while flowing the same solvent as the mobile phase for liquid chromatography. The mobile phase uses a mixture of acetonitrile: 10 mM acetic acid aqueous solution 60 to 80: 20 to 40 by weight. More preferably, the mixture is used in a 70:30 weight ratio. Desorption time is 4 ~ 6 minutes, 0.5 ~ 3mL / min flow at a flow rate of desorption. When the mobile phase is used, trichloroic acid, chlorophenols, and acidic pharmaceuticals have excellent separation efficiency, simultaneous analysis is possible, and a trace amount of 2 to 20ngL -1 can be analyzed.

상기 탈착된 용매를 액체크래마토그래피에 주입하고 UV 검출기를 이용하여 분석한다. 이때 액체크로마토그래피의 이동상은 상기 탈착용매와 동일한 용매인 아세토나이트릴 : 10mM 아세트산 수용액이 60 ~ 80 : 20 ~ 40 중량비로 혼합된 것을 사용하는 것이 바람직하다. 이동상의 유속은 0.5 ~ 3mL/min로 수행한다. 컬럼은 고정상으로 실리카가 충진된 것을 사용하며, 예를 들면 Luna C18 (250 x 4.6 mm i.d., 5 ㎛, Phenomenex, Torrance, CA, USA) 등을 사용할 수 있다. 이때 검출파장은 210 nm로 한다. 상기 고정상을 이용하는 경우 트리클로산, 클로로페놀류 및 산성의약품류의 분리효능이 우수하며, 동시 분석이 가능하고, 정량한계가 2 ~ 20ngL-1인 극미량도 분석을 할 수 있다.The desorbed solvent is injected into liquid chromatography and analyzed using a UV detector. At this time, the mobile phase of the liquid chromatography is preferably a mixture of acetonitrile: 10 mM acetic acid aqueous solution of 60 ~ 80: 20 ~ 40 weight ratio of the same solvent as the desorption solvent. The flow rate of the mobile phase is performed at 0.5 to 3 mL / min. The column uses a silica-filled bed as the stationary phase. For example, Luna C18 (250 × 4.6 mm id, 5 μm, Phenomenex, Torrance, CA, USA) may be used. The detection wavelength is 210 nm. In the case of using the stationary phase, trichloroic acid, chlorophenols and acidic pharmaceuticals have excellent separation efficiency, simultaneous analysis is possible, and a trace amount of 2 to 20ngL −1 can be analyzed.

본 발명에서 상기 클로로페놀류로는 3-클로로페놀, 2,4-클로로페놀이고, 2,4,6-클로로페놀 등을 포함하며, 산성 의약품류는 메페남산, 젬피브로질 등을 포함한다.In the present invention, the chlorophenols include 3-chlorophenol, 2,4-chlorophenol, and include 2,4,6-chlorophenol, and acidic medicines include mefenamic acid, gemfibrozil and the like.

본 발명은 물 중 미량으로 존재하는 유기물질인 트리클로산, 클로로페놀류, 산성 의약품류를 전처리 과정 중 유해한 유기용매의 사용과 유도체화 과정 없이 한 번의 추출 단계로 여러 가지 미량의 시료를 농축한 후 액체 크래마토그래피에 직접 주입하여 신속하게 물 중 유해 물질을 분석할 수 있다. The present invention concentrates various trace samples in a single extraction step without the use of harmful organic solvents and derivatization during the pretreatment process of triclosan, chlorophenols and acidic medicines, which are present in trace amounts, in the water. Direct injection into matographies allows rapid analysis of hazardous substances in water.

특히, 상기 CW/TPR 섬유와 이동상 및 고정상을 사용하여 미량의 트리클로산, 클로로페놀류 및 산성의약품류를 동시에 효과적으로 분석할 수 있다.In particular, the amount of triclosan, chlorophenols and acidic drugs can be effectively analyzed simultaneously using the CW / TPR fibers and the mobile and stationary phases.

이하는 본 발명의 구체적인 설명을 위하여 일예를 들어 설명하는 바, 본 발명이 하기 실시예에 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail with reference to the following examples. However, the present invention is not limited to the following examples.

[실시예 1]Example 1

막대자석을 넣은 유리병에 수집된 물 10 mL을 담은 후, CW/TPR 섬유 (carbowax/templated resine, 50 ㎛)를 넣어 물에 완전히 노출 시키고, 교반기 위에서 1000rpm으로 교반시키며 50 분간 추출을 수행하였다. 추출 과정을 거친 고체상 섬유는 전용 홀더를 이용하여 고체상 미량 추출법용 인터페이스에 장착 후 액체 크래마토그래피용 이동상(아세토나이트릴: 10mM 아세트산 수용액 70:30 중량비)으로 5분간 1mL/min의 유속으로 흘려주며 탈착시켰다. 탈착시킨 용액을 액체크마토그 래피의 UV 검출기를 이용하여 크래마토그램을 얻었다. 이때 액체크로마토그래피의 분석조건은 다음과 같다.After collecting 10 mL of collected water in a glass jar containing a bar magnet, CW / TPR fiber (carbowax / templated resine, 50 ㎛) was added to the water completely exposed, stirred at 1000rpm on a stirrer and extracted for 50 minutes. After the extraction process, the solid fiber is attached to the solid-phase micro-extraction interface using a dedicated holder, and then flows at a flow rate of 1 mL / min for 5 minutes in a liquid chromatographic mobile phase (acetonitrile: 70:30 weight ratio of 10 mM acetic acid aqueous solution). Desorbed. The desorbed solution was obtained by chromatogram using a UV detector of liquid chromatograph. At this time, the analysis conditions of the liquid chromatography are as follows.

-HPLC 컬럼: Luna C18 (250 x 4.6 mm i.d., 5 ㎛, Phenomenex, Torrance, CA, USA) HPLC column: Luna C18 (250 x 4.6 mm i.d., 5 μm, Phenomenex, Torrance, CA, USA)

-이동상: acetonitrile: aqueous 10 mM acetic acid (70:30, v/v, isocratic elution) at a flow rate of 1.0 mL/min. Mobile phase: acetonitrile: aqueous 10 mM acetic acid (70:30, v / v, isocratic elution) at a flow rate of 1.0 mL / min.

-검출파장: 210 nmDetection wavelength: 210 nm

그 결과는 도 1에 나타내었다. 도 1에 나타낸 바와 같이 트리클로산과 클로로페놀류, 산성 의약품류가 동시에 분석됨을 확인하였다. The results are shown in FIG. As shown in Figure 1, it was confirmed that triclosan and chlorophenols, acidic drugs are analyzed at the same time.

도 1은 본 발명의 시료 전처리법을 이용하여 분석된 크래마토그램이다. 도 1에서 1번 피크는 비스페놀이고, 2번 피크는 3-클로로페놀이고, 3번 피크는 2,4-클로로페놀이고, 4번 피크는 2,4,6-클로로페놀이고, 5번 피크는 메페남산이고, 6번 피크는 젬피브로질이고, 7번 피크는 트리클로산이다.1 is a chromatogram analyzed using the sample pretreatment method of the present invention. In Figure 1 peak 1 is bisphenol, peak 2 is 3-chlorophenol, peak 3 is 2,4-chlorophenol, peak 4 is 2,4,6-chlorophenol, peak 5 is Mephenamic acid, peak 6 is gemfibrozil, and peak 7 is triclosan.

Claims (4)

a) 물에 함유된 트리클로산, 클로로페놀류, 산성 의약품류를 CW/TPR(carbowax/templated resine) 섬유로 흡착하는 단계;a) adsorbing triclosan, chlorophenols and acidic medicines contained in water with carbowax / templated resine (CW / TPR) fibers; b) 상기 CW/TPR 섬유를 액체 크로마토그래피용 이동상과 동일한 용매에 접촉하여 흡착된 추출물을 탈착하는 단계; 및b) contacting the CW / TPR fibers with the same solvent as the mobile phase for liquid chromatography to desorb the adsorbed extract; And c) 상기 탈착된 용액을 액체크로마토그래피를 이용하여 분석하는 단계;c) analyzing the desorbed solution using liquid chromatography; 를 포함하는 물에 함유된 트리클로산, 클로로페놀류, 산성 의약품류의 동시 분석방법.Simultaneous analysis of triclosan, chlorophenols, acidic medicines contained in water. 제 1항에 있어서,The method of claim 1, 상기 이동상은 아세토나이트릴 : 10mM 아세트산 수용액이 60 ~ 80 : 20 ~ 40 중량비로 혼합된 것을 사용하는 물에 함유된 트리클로산, 클로로페놀류, 산성 의약품류의 동시 분석방법.The mobile phase is a method for the simultaneous analysis of triclosan, chlorophenols, acidic medicines contained in water using acetonitrile: 10mM acetic acid aqueous solution mixed in a 60 to 80: 20 to 40 weight ratio. 제 2항에 있어서,3. The method of claim 2, 상기 액체 크로마토그래피의 고정상은 실리카인 물에 함유된 트리클로산, 클로로페놀류, 산성 의약품류의 동시 분석방법.The fixed phase of the liquid chromatography is a simultaneous analysis of triclosan, chlorophenols, acidic medicines contained in water silica. 제 1항에 있어서,The method of claim 1, 상기 a)단계에서 물의 온도는 23 ~ 25℃, pH 범위는 2 ~ 4이며, 추출시간은 10 ~ 60분인 물에 함유된 트리클로산, 클로로페놀류, 산성 의약품류의 동시 분석방법.The temperature of the water in step a) is 23 ~ 25 ℃, pH range is 2 to 4, extraction time is 10 to 60 minutes, simultaneous analysis of triclosan, chlorophenols, acidic medicines contained in water.
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CN104820053A (en) * 2015-05-06 2015-08-05 宁波市海洋与渔业研究院 Method of measuring nineteen chloro-phenols and sodium salt thereof in aquatic animals through gas chromatography-mass spectrography (GC-MS) method
CN113252815A (en) * 2021-06-16 2021-08-13 中国科学院地理科学与资源研究所 Method for detecting triclosan and triclocarban in sludge compost
CN117147720A (en) * 2023-08-30 2023-12-01 阳江市检测检验中心 Method for detecting triclosan and triclocarban in vegetables

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JPS5576949A (en) 1978-12-06 1980-06-10 Showa Denko Kk Acidic substance analyser by means of high speed liquid chromatograph
JP2008185373A (en) 2007-01-26 2008-08-14 Suntory Ltd Method of analyzing acidic oligosaccharide-containing sugar composition

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104820053A (en) * 2015-05-06 2015-08-05 宁波市海洋与渔业研究院 Method of measuring nineteen chloro-phenols and sodium salt thereof in aquatic animals through gas chromatography-mass spectrography (GC-MS) method
CN113252815A (en) * 2021-06-16 2021-08-13 中国科学院地理科学与资源研究所 Method for detecting triclosan and triclocarban in sludge compost
CN117147720A (en) * 2023-08-30 2023-12-01 阳江市检测检验中心 Method for detecting triclosan and triclocarban in vegetables

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