• Archives of Pharmacal Research
• /
• 제15권2호
• /
• pp.109-114
• /
• 1992

For the risk assessment of human exposure to volatile halogenated hydrocarbons, a dynamic purge trap/on-column cryofocusing method using capillary gas chromatograph-$^{63}Ni$ electron capture detector and thermal desorption unit was applied to analyze the free forms, metabolites of 1, 1, 2-trichloroethylene and 1, 1, 2, 2-tetrachloroethylene. The urine sample was diluted with distilled water, hydrolyzed and sealed. Then the inert gas was infused to purge out free 1, 1, 2-trichloroethylene, free 1, 1, 2, 2-tetrachloroethylene and urichloroethanol. These compounds were trapped to $Tenax^R$ / GC-gas trap device throughout clean up tube. Being undertectable to gas chromatograph directly, trichloroacetic acid was methyl esterificated and trapped in the manner above mentioned. The optimal incubation time to get best recovery of methyl ester was 4 hours at $60^circ$C. The concentrations of free volatile halogenated hydrocarbons and their metabolites in urine were obtained of free volatile halogenated hydrocarbons and their metabolites in urine were obtained from 5 healthy volunteers. This analytical method is expected to make the biological monitoring more precise and convenient.

• 대한의용생체공학회:의공학회지
• /
• 제37권1호
• /
• pp.31-38
• /
• 2016

For the patients with bladder dysfunction, measurement of urine volume inside the bladder is very critical to avoid bladder failure. In measuring urine volume inside a bladder, low-resolution 3D ultrasound images are widely used. However, urine volume estimation from 3D ultrasound images is prone to big errors and inconsistency because of low spatial resolution and low signal-to-noise ratio of ultrasound images. We developed a new robust volume estimation algorithm which is not computationally expensive. We tested the algorithm on a lab-built ultrasound bladder phantom and volunteers. The average error rate of the human bladder volume estimation was 5.9% which was better than the commercial machine.

• 한국지하수토양환경학회지:지하수토양환경
• /
• 제21권1호
• /
• pp.28-39
• /
• 2016

Struvite (MgNH₄PO₄ ⋅ 6H₂O) and hydroxyapatite (HAP, Ca₁₀(PO₄)₆(OH)₂) precipitation in urine-separating toilets (NoMix toilets) causes severe maintenance problems and also reduce the phosphate and calcium content. Application of urine separating technique and extraction of by-products from human urine is a cost effective technique in waste water treatment. In this study, we extract urine calcite from human urine by batch scale method, using urease producing microbes to trigger the precipitation and calcite formation process. Extracted urine calcite (calcining at 800℃) is a potential adsorbent for removal of heavy metal(loid)s like (Cd²⁺, Cu²⁺, Ni²⁺, Pb²⁺, Zn²⁺ and As³⁺) along with additional leaching analysis of total nitrogen (T-N), phosphate (T-P) and chemical oxygen demand (COD). The transformations of calcite during synthesis were confirm by characterization using XRD, SEM-EDAX and FT-IR techniques. In additional, the phosphate leaching potential and adsorbate (nitrate) efficiency in aqueous solution was investigated using the calcinedurine calcite. The results indicate that the calcite was effectively remove heavy metal(loid)s lead up to 96.8%. In addition, the adsorption capacity (q_e) of calcite was calculated and it was found to be 203.64 Pb, 110.96 Cd, 96.02 Zn, 104.2 As, 149.54 Cu and 162.68 Ni mg/g, respectively. Hence, we suggest that the calcite obtain from the human urine will be a suitable absorbent for heavy metal(loid)s removal from aqueous solution.

• Bulletin of the Korean Chemical Society
• /
• 제31권8호
• /
• pp.2322-2328
• /
• 2010

A multiple solid-phase extraction (SPE) method was used with liquid chromatography, coupled with mass spectrometry (LC/MS), for the analysis of heterocyclic amines (HCAs) in human urine. Separation efficiencies based on the pH of the mobile phase and the types of columns were compared. An amide column showed better baseline separation and narrower HCA peak widths at pH 5.0 for the mobile phase than a $C_8$ column. Each SPE step, HLB, MCX, and HybridSPE, was optimized by controlling the pH conditions. The combined method with the three SPEs effectively removed interfering species that cause ion-suppression during HCA detection. Validation of the method, performed with SIM and SRM detection, showed correlation coefficients above 0.991 in the range 0.3 - 16.7 ng/mL. Recovery rates were 45.4 - 97.3% on the $C_8$ column and 71.8 - 101.4% on the amide column, and method detection limits were 0.11 - 0.65 ng/mL on the $C_8$ column and 0.12 - 0.48 ng/mL on the amide column. This method using multiple SPEs offers significant benefits for high-throughput determination of HCAs in urine.

• 분석과학
• /
• 제11권3호
• /
• pp.167-173
• /
• 1998

Electrothermal Vaporization-Hollow Cathode Glow Discharge-Atomic Emission Spectrometer(ETV-HCGD-AES)를 이용하여 혈청과 뇨에 함유된 중금속 원소들의 분석을 시도하였다. 먼저 글로우 방전셀을 목적에 맞게 설계하고, 미국 NIST로부터 구입한 표준시료인 혈청과 뇨를 사용하여 미량분석을 위한 기초실험을 수행하였다. 전처리를 하지 않은 시료의 분석에서 새로이 개발한 ETV-HCGD-AES는 수은이나 납 등의 검출에서 ICP-OES보다 상대적으로 전처리가 거의 필요없었으며 감도와 선택성에서도 우수함을 관찰하였다.

• 약학회지
• /
• 제57권5호
• /
• pp.330-336
• /
• 2013

"The Act on Medication Treatment of Sexual Impulse of Sex Offenders" known as chemical castration has been effective since July 2011 in Korea. According to the law, monitoring of male sex hormone in urine is enforced to request National Forensic Service more than once a month after injection of medicine designed to reduce sex impulse. We established a rapid and sensitive method for the monitoring of testosterone (T) and epitestosterone (E) in human urine by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Three mL of urine was pretreated by solid-phase extraction for purification and performed enzymatic hydrolysis. The pretreated samples were extracted twice with 2 ml of ethyl acetate and n-hexane (2 : 3). The separation was applied on Thermo Hypersil GOLD C18 column ($1.9{\mu}m$, $100{\times}2.1mm$). A gradient elution of methanol and water of 0.1% formic acid were used as mobile phase and the retention time was less than 10 min. LC-MS/MS system coupled with an electrospray ionization source was performed in multiple reaction monitoring mode. The transitions of the analytes executed as following: m/z $289{\rightarrow}97$, 109 for T and E, m/z $292{\rightarrow}109$ for $T-d_3$ and $E-d_3$ as internal standards. The validation results of the method were satisfactory. The limits of detection were 0.05 ng/ml and the limits of quantification were 0.1 ng/ml. This method was successfully applied to real human urine sample. The developed method will be useful for monitoring T/E ratio in urine of sex offenders.

• Asian Pacific Journal of Cancer Prevention
• /
• 제17권3호
• /
• pp.1083-1088
• /
• 2016

Background: Cervical cancer is the second commonest cancer among Indian women and its association with human papilloma virus (HPV) is well established. This preventable cancer accounts for the maximum number of cancer related deaths among rural Indian women. Unlike in developed countries there are no organized cervical cancer screening programmes in India due to lack of resources and manpower. Objective: To detect genital HPV infection using urine samples among asymptomatic rural women in the age group of 18-65 years. Materials and Methods: The study area chosen was Perdoor village in Udupi Taluk, Karnataka State and all the women in the age group of 18-65 years formed the study cohort. A cross sectional study was conducted by house visits and 1,305 women were enrolled in the study. After taking written informed consent a data sheet was filled and early stream random urine samples were collected, transported to a laboratory at 4OC and aliquoted. Samples were tested using nested HPV PCR with PGMY09/11 and GP5+/6+ primers. Positive cases were genotyped by sequence analysis. Results: Study participants included 1,134 sexually active and 171 unmarried women with a mean age at marriage of 22.1 (SD=3.9) years. Study area showed high female literacy rate of 86.6%. Five urine samples tested positive for HPV DNA (0.4%). Conclusions: We found very low genital HPV infection rate among women from monogamous community. This is the first major population based study carried out among asymptomatic rural women to detect genital HPV infectio from Karnataka using urine samples.

• 약학회지
• /
• 제57권6호
• /
• pp.420-425
• /
• 2013

Phentermine (PT) and phenmetrazine (PM) have been widely used as anti-obesity drugs. These drugs should be used with caution due to its close relation to amphetamine in its structure and toxicity. PT and PM, amphetamine-type anorectics, have recently been considered as alternatives for methamphetamine abuse in Korea. In addition, the misuse and abuse of PT and PM obtained by illegal sources such as the internet become a serious social problem. In the present study, a simultaneous detection and quantification method for determining PT and PM in human urine was developed and validated according to the international guidelines. The urine samples were screened using a fluorescence polarization immunooassay and analyzed by gas chromatography mass spectrometry (GC-MS) after extraction using automatic solid phase extraction (SPE) with a mixed-mode cation exchange cartridge and derivatization with pentafluoropropionic anhydride (PFPA). The validation results for selectivity, linearity, limits of detection (LOD) and quantification (LOQ), intra- and inter-assay precision and accuracy and recovery were satisfactory. The validated method was successfully applied to authentic urine samples collected from 38 drug abuse suspects. PT and/or PM were identified with or without methamphetamine in urine samples. Abuse of PT and PM have increased continuously in Korea, therefore, closer supervision of the inappropriate use of anoretics is necessary.

• 분석과학
• /
• 제32권5호
• /
• pp.163-172
• /
• 2019

Methamphetamine (MA) is currently the most abused illicit drug in Korea and its major metabolite is amphetamine (AP). As MA exist as two enantiomers with the different pharmacological properties, it is necessary to determine their respective amounts in a sample. Thus a chiral stationary phase liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for identification and quantification of d-MA, l-MA, d-AP, and l-AP in human urine. Urine sample ($200{\mu}L$) was diluted with pure water and purified using solid-phase extraction (SPE) cartridge. A $5-{\mu}L$ aliquot of SPE treated sample solution was injected into LC-MS/MS system. Chiral separation was carried out on the Astec Chirobiotic V2 column with an isocratic elution for each enantiomer. Identification and quantification of enantiomeric MA and AP was performed using multiple reaction monitoring (MRM) detection mode. Linear regression with a $1/x^2$ as the weighting factor was applied to generate a calibration curve. The linear ranges were 25-1000 ng/mL for all compounds. The intra- and inter-day precisions were within 3.6 %, while the intra- and inter-day accuracies ranged from -5.4 % to 11.8 %. The limits of detection were 2.5 ng/mL (d-MA), 3.5 ng/mL (l-MA), 7.5 ng/mL (d-AP), and 7.5 ng/mL (l-AP). Method validation parameters such as selectivity, matrix effect, and stability were evaluated and met acceptance criteria. The applicability of the method was tested by the analysis of genuine forensic urine samples from drug abusers. d-MA is the most common compound found in urine and mainly used by abusers.

• 분석과학
• /
• 제24권3호
• /
• pp.183-192
• /
• 2011

본 연구에서는 LC/ESI/MS 및 GC/MS로 superdrol을 인체에 경구투여 한 후 채취한 요시료 중에 함유된 superdrol 및 그 대사체의 분석법을 확립하고 이들의 체내 배설형태를 조사하였다. 액체-액체 추출에서 최적 추출 pH는 6.5 이고 최적 추출 용매는 diethly ether이였다. GC/MSD를 이용하여 superdrol과 그 대사체의 분석법에 대한 유효성을 점검한 결과, intra-day의 회수율은 89.7-113.2%, 정확도 91.8-113.8%, 재현성은 0.2-6.8%로 나타났고 inter-day의 회수율은 89.3-104.1%, 정확도는 95.2-103.0%, 재현성은 0.7-7.8%로 나타났다. LC/ESI/MS을 통해 얻은 blank urine과 dosed urine의 크로마토그램을 비교하여 superdrol의 대사체를 검출하였으며 Superdrol과 그 대사체를 유도체화 시켜 GC/TOF-MS로 확인하였다. 확보된 질량스펙트럼으로부터 superdrol M1의 경우 superdrol의 3-C 위치의 케톤기가 하이드록시기로 환원된 것으로 추정할 수 있었고 M2의 경우 superdrol의 D-ring에 하이드록시기가 첨가된 것으로 추정할 수 있었다. 또한, 효소가수분해과정을 비교해 본 결과 superdrol과 그 대사체들은 대부분 글루쿠론산 포합체를 형성하여 체외로 배설되는 것을 확인하였다. Superdrol 경구투여 후 채취한 요시료로부터 superdrol과 그 대사체의 배설양상을 조사한 결과, 모두 4.3 시간에서 최대배설량을 보였고 superdrol과 superdrol M1은 48시간까지도 미량검출 되어 체내 잔류성이 높은 물질임을 확인할 수 있었다.