• 한국식품영양과학회지
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• 제28권6호
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• pp.1208-1211
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• 1999

Semi HPLC using a column switching technique was used to determine the trace content of vitamin B12 in various foods. Total analytical time required less than 20 mins per sample and the recovery ratio was 99.9, 99.6, 100.1 and 99.8% for 1.0, 10.0, 100.0 and 1,000 g/kg, respectively. The content of vitamin B12 in various foods obtained using column switching method showed higher levels compared to labels in dried milk(0.5 g/100g) and in grain products(0.51~34.36 g/100g). Thus, this column switching method was more sensitive, effective and precise than the microbiological analysis currently used to determine the trace compounds like a vitamin B12.

• 대한화학회지
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• 제39권4호
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• pp.257-265
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• 1995

시중에 시판되고 있는 우유를 전처리하여 이 우유에 포함된 유리 아미노산을 dansyl-chloride로 유도체화시켜 C-18 컬럼을 이용한 역상 LC법으로 분리한 다음 표준물 첨가법으로 정량했다. 미량의 D-아미노산의 분리에서는 LC의 Column-Switching System을 이용하였으며 비키랄 컬럼을 통과한 단실 D/L-아미노산에 $Cu(N-benzyl-L-proline)_2$를 이동상에 첨가한 키랄 분리를 수행하여 L-아미노산에서 D-아미노산을 분리 정량했다. 이 방법은 우유시료 중에 존재하는 16가지 아미노산의 정량이 가능하며 이중에 12가지의 D-아미노산이 column switching 방법을 통한 키랄 분리로 정량이 가능하다. 우유 100 mL에 총 유리 아미노선이 41.00 mg 포함되어 있음을 확인했으며, D-아미노산은 D-glutamic acid가 2.05%, D-alanine 2.93%만이 포함되어 있음을 확인했다.

• Archives of Pharmacal Research
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• 제17권6호
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• pp.458-461
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• 1994

A new high-performance liquid chromatographic method with column switching has been onto a Bondapak phenyl/corsil $(37-50{\;}{\mu}m)$ precolumn and polar plasma components were washed with 0.06 M borate burffer. After valve switching, the concentrated drug were eluted in the back-flush mode and separated on a ${\mu}-Bondapak$ C18 column with acetonitrilke-phosphate buffer as the mobile phae. The method showed excellent precision, accuracy and speed with detection limit of $0.01{\;}{\mug}/ml^{-1}$. Total analysis time per smaple was less than 20 min and the coefficients of variation for intra and inter-assay were less than 5.635. This method has been successfully applied to plasma smaples from eats after oral administration of omeprazole.

• Journal of Pharmaceutical Investigation
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• 제30권1호
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• pp.51-54
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• 2000

A column-switching high performance liquid chromatographic method has been developed for the determination of a fluconazole in human plasma. Each plasma sample was centrifuged for 10 min at 5000 g. After an aliqout of the supernatant was taken to nylon microcentrifuge filter, these samples were centrifuged for 10 min at 5000 g. An aliqout of the supernatant was injected directly onto the HPLC column. Deionized water was run for 2 min at a flow rate of 1.0 ml/min to retain fluconazole in an extration column, while proteins and endogenous interferences were eluted to the waste. The analyte was then back-flushed onto an analytical column, $C_{18}$ reversed-phase column. The mobile phase for analytical column, 0.01 M sodium acetate (pH 5.0)-methanol (65:35, v/v), was run at a flow rate of 1.0 ml/min. The column effluent was monitored by ultraviolet detection at 261 nm. The retention time for fluconazole was 11.76 min in human plasma. The detection limit for fluconazole in human plasma was $0.2\;{\mu}g/ml$. No interference from endogenous substances was observed.

• 한국식품과학회지
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• 제37권6호
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• pp.1024-1027
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• 2005

본 연구에서는 성장기용 조제식 중에 영양강화를 위해 첨가하는 비타민 $D_3$와 $K_1$의 함량측정을 위해 lipase를 이용하여 효소 가수분해 후 유기용매로 비타민을 추출하여 동시에 분석하는 신속분석법을 위와 같이 수행하였다. 추출된 비타민을 전처리 컬럼에서 2번의 switching time을 설정하여 농축컬럼에 홉착시킨 후 gradient mode로 2가지 이동상으로 분석컬럼에서 각각의 성분을 모두 분리하여 동시에 검출하는 방법을 사용하였다. 시료로 사용된 성장기용 조제식은 표기함량보다 다소 높게 분석되었으나, 국제표준인증물질을 시료로 사용하여 본 연구의 실험방법에 의해 측정된 값은 인증된 표준값내의 결과를 보여주었다. 따라서, 비타민 $D_3$ 또는 $K_1$을 강화한 분유, 이유식 등의 분말 유제품 중에서 함량을 측정하고자 할 때 한정된 장비와 인력으로 각각의 2가지 실험방법을 수행하기가 어렵거나 시간단축이 필요한 경우, 본 연구에서 수행한 실험방법과 같이 시료전처리를 간단하고 신속하게 수행할 뿐만 아니라 역상컬럼과 column-switching HPLC에 의해 비타민 $D_3$ 또는 $K_1$을 동시에 분석함으로써 보다 효율적인 분석을 진행 할 수 있을 것으로 사료된다.

• Archives of Pharmacal Research
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• 제21권2호
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• pp.212-216
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• 1998

A coupled achiral-chiral high-performance liquid chromatographic system has been developed for the determination of the enantiomers of salmeterol, S-(+)-salmeterol and R-(-)-salmeterol in urine. THe salmeterol was separated from the interfering components in urine and quantified on the silica column, and the enantiomeric composition was determined on a Sumichiral OA-4700 chiral stationary phase. The two columns were connected by a switching valve equipped with a silica precolumn. The two columns wer connected by a switching valve equipped with a silica precolumn. The precolumn was used to concentrate the salmeterol in the eluent from the achiral column before backflushing onto the chiral phase. The coupled system was validated.

• Archives of Pharmacal Research
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• 제24권3호
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• pp.207-210
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• 2001

A fully automated high performance liquid chromatography with column-switching was developed for the simultaneous determination of KR60436, a new reversible proton pump inhibitor, and its active metabolite O-Demethyl-KR60436 from rat plasma samples. Plasma sample (50$\mu$l) was directly introduced onto a Capcell Pak MF Ph-1 column ($10{\times}4$ mm I.D.) where primary separation was occurred to remove proteins and concentrate target Substances Using acetonitrile-Potassium Phosphate (PH 7, 0.1 M) (2 : 8, v/v). The drug molecules eluted from MF Ph-1 column were focused in an intermediate column ($10{\times}2$ I.D.) by the valve switching step. The substances enriched in intermediate column were eluted and separated on a Vydac 218MR53 column ($250{\times}3.2$ I.D.) using acetonitrilepotassium phosphate (pH 7, 0.02 M) (47:53, v/v) at a flow rate of 0.5 ml/min when the valve status was switched back to A position. The method showed excellent sensitivity (detection limit of 2 ng/ml) with small volume of samples ($50{\mu}$l), good precision and accuracy, and speed (total analysis time 24 min) without any loss in chromatographic efficiency. The response was linear ($r^2{\geq}0.797$) over the concentration range of 5-500 ng/ml.

• Archives of Pharmacal Research
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• 제17권5호
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• pp.360-363
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• 1994

Column--swtiching technique with a reversed-phase high performance liquid chromatographic method has been developed for the routine analysis of radioiodinated insulin and its degadation products in biological fluids. The diluted biological samples were loaded onto a precolumn packed with LiChrosorb RP-8 $(25-40{\;}{\mu}m)$ using 0.1% trifuoroacetic acid (TFA) in water as a washing solvent. After valve switching, the concentrated insulins were eluted in the back-flush mode and separated by a W-Porex $C_{18}$ column with a gradient of 0.1% TFA in water and 0.1% TFA in acetonitrile as the mobile phase. The method showed good precision, accuracy and speed with the detection limit of 20 pg/ml. Total analysis time per sample was about 40 min and the coefficients of variation were less than 8, 2%.

• 대한약학회:학술대회논문집
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• 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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• pp.398.2-398.2
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• 2002

A column switching HPLC assay was developed to allow the separation and quantitation of cetirizine in human plasma by ultraviolet (UV) detection. Plasma samples were prepared by liquid-liquid extraction. After drying, the residue was reconstituted in 20 mM phosphate buffer (pH 2.8) containing 15% acetonitrile. The samples were initially injected onto a clean-up Capcell Pak MF C18 column. (50 mm $\times$ 4.6 mm I.D.), and the chromatographic region containing the peaks of interest was followed in an analytical C18 microcolumn (250 mm$\times$1.5 mm I. D.) via column switching device. (omitted)

• Archives of Pharmacal Research
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• 제23권5호
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• pp.441-445
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• 2000

Achiral-chiral column switching HPLC assay was developed to allow the separation and quantification of the enantiomers of terbutaline in human plasma by means of fluorescence detection. Plasma samples were prepared by solid-phase extraction with sep-pak silica, followed by HPLC assay. The enantiomers of terbutaline and the internal standard were separated from the biological matrix on a silica column, and the two enantiomers were resolved and quantified on a Sumichiral OA-4900 column. The two columns were connected by a switching valve equipped with silica trap column, The trap column was used to concentrate the terbutaline in the eluent from the achiral column before back flushing onto the chiral phase. For each enantiomers, the assay was linear between 2.5-125 ng/$m\ell$ (r=0.9999) and detection limit was 1.0 ng/$m\ell$ .