• Title, Summary, Keyword: Single residual analytical method

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Analytical Method Development and Monitoring of Residual Solvents in Dietary Supplements (건강기능식품 중 잔류용매 분석법 개발 및 모니터링)

  • Lee, Hwa-Mi;Shin, Ji-Eun;Jang, Young-Mi;Kim, Hee-Yun;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.42 no.4
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    • pp.390-397
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    • 2010
  • Residual solvents in foods are defined as organic volatile chemicals used or produced in manufacturing of extracts or additives, or functional foods. The solvents are not completely eliminated by practical manufacturing techniques and they also may become contaminated by solvents from packing, transportation or storage in warehouses. Because residual solvents have no nutritional value but may be hazardous to human health, there is a need to remove them from the final products or reduce their amounts to below acceptable levels. The purpose of this study was to develop and evaluate an analytical method for the screening of residual solvents in health functional foods. Furthermore, the aim of this study was to constitute a reasonable management system based on the current state of the market and case studies of foreign countries. Eleven volatile solvents such as MeOH, EtOH, trichloroethylene and hexane were separated depending on their column properties, temp. and time using Gas Chromatography (GC). After determining the GC conditions, a sample preparation method using HSS (Head Space Sampling) was developed. From the results, a method for analyzing residual solvents in health functional foods was developed considering matrix effect and interference from the sample obtained from the solution of solvents-free health functional foods spiked with 11 standards solutions. Validation test using the developed GC/HSS/MS (Mass Spectrometry) method was followed by tests for precision, accuracy, recovery, linearity and adequate sensitivity. Finally, examination of 104 samples grouped in suits was performed by the developed HSS/GC/MS for screening the solvents. The 11 solvents were isolated from health functional foods based on vapor pressure difference, and followed by separation within 15 minutes in a single run. The limt of detection (LOD), limit of quantification (LOQ), recovery and coefficient of variation (C.V.) of these compounds determined by the HSS/GC/MS were found to be 0.1 pg/mL, 0.1-125 pg/g, 51.0-104.6%, and less than 15%, respectively. Using the developed HSS/GC/MS method, residual solvent from 16 out of 104 health functional products were detected as a EtOH. This method therefore seems t o be a valuable extension ofanalytical method for the identification of residual solvents in health functional food.

Method Development and Validation for Analysis of Isopyrazam Residues in Agricultural Products (농산물 중 살균제 Isopyrazam의 개별 잔류분석법 확립)

  • Kim, Ji-Yoon;Kim, Ja-Young;Ham, Hun-Ju;Do, Jung-Ah;Oh, Jae-Ho;Lee, Young-Deuk;Hur, Jang-Hyun
    • The Korean Journal of Pesticide Science
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    • v.17 no.2
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    • pp.84-93
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    • 2013
  • Validated analytical methods for isopyrazam are meager or lacking. In the present study, a single residual analytical method was developed for isopyrazam in selected commodities. Isopyrazam was analyzed in brown rice, soybean, green pepper, mandarin, cucumber, and Korean melon. We tried different solvents and methods through extraction, partition and purification steps to obtain best analytical results. For isopyrazam samples were extracted with acetonitrile, concentrated and partitioned with n-hexane, clean-up using florisil with n-hexane/ethylacetate (70/30) and analyzed with HPLC/UVD. The limit of quantitation (LOQ) for isopyrazam was 1.0 ng (S/N > 10) and method LOQ (MLOQ) was 0.04 mg $kg^{-1}$. Recovery ranged through 81.0~105.3% (syn-isomer) and 80.8~105.6% (anti-isomer) at fortification level of 0.04 (MLOQ), 0.4 (10 ${\times}$ MLOQ), and 2.0 (50 ${\times}$ MLOQ). The coefficient of variation (CV) for isopyrazam was less than 10% regardless of sample types. These results were further confirmed with LC/MS, respectively. The proposed method is highly reproducible and sensitive and is suitable for routine analysis.

Actuator Fault Detection and Isolation Method for a Hexacopter (헥사콥터의 구동기 고장 검출 및 분리 방법)

  • Park, Min-Kee
    • Journal of IKEEE
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    • v.23 no.1
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    • pp.266-272
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    • 2019
  • Multicopters have become more popular since they are advantageous in their ability to take off and land vertically. In order to guarantee the normal operations of such multicopters, the problem of fault detection and isolation is very important. In this paper, a new method for detecting and isolating an actuator fault of a hexacopter is proposed based on the analytical approach. The residual is newly defined using the angular velocities of actuators estimated by the mathematical model and an actuator fault is detected comparing the residuals to a threshold. And a fault is isolated combining a dynamic model and generated residuals when a fault is detected. The proposed method is a simple, but effective technique because it is based on mathematical model. The results of the computer simulation are also given to demonstrate the validity of the proposed algorithm in case of a single failure.

Active Vibration Control of Slewing Smart Beam (회전지능보의 능동진동제어)

  • Nam, Sang-Hyun;Kwak, Moon-Kyu
    • Proceedings of the Korean Society for Noise and Vibration Engineering Conference
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    • pp.257-262
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    • 2000
  • This research is concerned with the active vibration control of slewing smart structures subjected to rotating disturbance. When cantilever beam rotates about axes perpendicular to the undeformed beam's longitudinal axis, it experiences inertial loading. Hence, the beam vibrates after the slewing ends. In this paper, the analytical model for a single slewing flexible beam with surface bonded piezoelectric sensor and actuator is developed using the Hamilton's principle with discretization by the assumed mode method. The theoretial model is verified by the experimental open loop frequency response data. The controller is designed for residual vibration suppression after slewing. The designed cotroller is a positive position feedback (PPF) controller for controlling the first mode vibration.

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Separation and recovery of semi-volatile substances of Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus by reduced pressure collections and GC-MS

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.33 no.1
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    • pp.11-22
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    • 2020
  • When extracting semi-volatile components of herbal medicines using hot water vapor, some substances may react with water vapor or oxygen, and some volatile substances may be lost, when using an organic solvent extraction method has the disadvantage that it may contain a non-volatile material and residual organic solvent. In addition, it is inefficient to separate semi-volatile substances from herbal medicines into each single component and conduct biological activity research for each component to determine the effective ingredient, and some components may be lost in the separation process. In this study, semi-volatile substances evaporated under two pressure-reduced conditions in Chinese herbal medicines such as Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were separated by cooling with liquid nitrogen. Those were analyzed by gas chromatography-mass spectrometry (GC-MS) to identify the components, and this method may be used to study biological activities at the cellular level. The substances separated under reduced pressure, essential oil obtained by simultaneous distillation extraction (SDE) method and substances by using solid phase micro-extraction (SPME) from Cnidii Rhizoma, Aucklandiae Radix and Amomum Fructus were analyzed by GC-MS. In the case of Cnidii Rhizoma and Aucklandiae Radix, there were some differences among the essential oil components obtained by SDE and those identified by low temperature capture (CT) and SPME method, these were believed to be produced by some volatiles reacting with water or oxygen at the boiling point temperature of water.

A Study on the Valid Dynamic Modeling for the Slewing and Vibration Suppression Control of Beam (보의 회전 및 진동제어를 위한 동적 모델 타당성 연구)

  • 곽문규;남상현
    • Journal of KSNVE
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    • v.11 no.2
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    • pp.292-300
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    • 2001
  • This research is concerned with the validation of the modeling technique and controller design for slewing beam structures. When cantilever beam rotates about axes perpendicular to the undeformed beam's longitudinal axis, it experiences inertial loading. Hence, the beam vibrates from the initial stage of slewing. In this paper, the analytical model for a single slewing flexible beam with surface bonded piezoelectric sensor and actuator is developed using the Hamilton's principle with discretization by the assumed mode method. Comparisons with the theoretical model are made based upon the frequency responses and time responses. A new factor called the coupling coefficient is introduced to incorporate the discrepancies between the theoretical and experimental results. The slewing is achieved by applying the PID control, which is found to be less sensitive to vibrations. The vibrations are controlled by PPF controller, which is found to be effective in suppressing residual vibrations after slewing. The vibrations occurred during slewing is difficult to control because the piezoceramic actuator is not powerful enough to overcome inertial loadings.

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An Elastic-Plastic Stress Analysis in Silicon Carbide Fiber Reinforced Magnesium Metal Matrix Composite Beam Having Rectangular Cross Section Under Transverse Loading

  • Okumus, Fuat
    • Journal of Mechanical Science and Technology
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    • v.18 no.2
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    • pp.221-229
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    • 2004
  • In this work, an elastic-plastic stress analysis has been conducted for silicon carbide fiber reinforced magnesium metal matrix composite beam. The composite beam has a rectangular cross section. The beam is cantilevered and is loaded by a single force at its free end. In solution, the composite beam is assumed perfectly plastic to simplify the investigation. An analytical solution is presented for the elastic-plastic regions. In order to verify the analytic solution results were compared with the finite element method. An rectangular element with nine nodes has been choosen. Composite plate is meshed into 48 elements and 228 nodes with simply supported and in-plane loading condations. Predictions of the stress distributions of the beam using finite elements were overall in good agreement with analytic values. Stress distributions of the composite beam are calculated with respect to its fiber orientation. Orientation angles of the fiber are chosen as $0^{circ},\;30^{circ},\;45^{circ},\;60^{circ}\;and\;90^{circ}$. The plastic zone expands more at the upper side of the composite beam than at the lower side for $30^{circ},\;45^{circ}\;and\;60^{circ}$ orientation angles. Residual stress components of ${\sigma}_{x}\;and \;{\tau}_{xy}$ are also found in the section of the composite beam.

An investigation of lead absorption in an electric accumulator factory with the use of personal samplers

  • Williams M.K.;King E.;Walford Joan
    • 대한예방의학회:학술대회논문집
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    • pp.561-575
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    • 1994
  • Williams, M K., King, E., and Walford, Joan (1969). Brit. J. industr. Med., 26, 202-216. An investigation of lead absorption in an electric accumulator factory with the use of personal samplers. Thirty-nine lead workers and controls, in stable conditions of exposure, each wore personal lead-in-air samplers daily for two weeks. During the second week samples for blood lead, urinary lead, urinary coproporphyrin, urinary $\gamma$-aminolevulinic acid (ALA), the punctate basophil count, and haemoglobin were taken daily. Duplicate estimations were made on one day. The lead exposures of men doing almost identical jobs differed by ratios of up to four to one. This could be attributed on y to personal differences in working habits. The correlation coefficients and regression equations of the biochemical tests with lead-in-air and with each other were determined. The mean values and $95\%$ confidence limits of single determinations of some of the biochemical tests corresponding to the two commonly accepted TLVs of lead-in-air (0-20 and 0-15 mg./$m^{3}$) were calculated from the regression equations. For each biochemical test the variation due to analytical error, the variation from day to day within subjects and the residual variation about the regression on lead-in-air were calculated. Previous estimates of the latter are not known. Excessive confidence may be placed in an index of exposure due to its low coefficient of variation within subjects unless the coefficient of variation between subjects about regression is taken into account. The correction for specific gravity of estimations of lead and ALA in spot samples of urine was found to reduce slightly the residual variation between subjects about the regression on lead-in-air and to increase the correlations with lead-in-air and with the other biochemical tests, but these changes were not statistically significant. The modified method used for estimating blood lead and urinary lead is described and validated.

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An experimental study on the comparison of trace amount of sulfonamides detection method in raw milk. (원유중 미량 설파제 검출방법 비교에 대한 실험적 연구)

  • 황원무;이성모;손봉환;이원창
    • Korean Journal of Veterinary Service
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    • v.20 no.1
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    • pp.79-93
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    • 1997
  • The sulfonamide is one of potentiative antimicrobial agents which is being used widely in veterinary medicine for control of several animal diseases such as mastitis as well as for promotion of growth. However, the misusages of sulfonamides in food producing animals, especially cattle produce several considerable problems in human health caused from residues of this antibiotic in milk product. To determine the most effective analytical methods for residual sulfonamides in raw milk, this study was performed comparatively using by some applicable screening detecting method such as TTC, Charm II test (sulfonamides), and Lactek tests (sulfamethazine kit). The positive result from screening tests was confirmed by HPLC method. Milk samples (540 raw milks) were collected from dairy farms. Results of this study are summariezed as follorrs ; 1. All samples (540 raw milks) showed negative response from TTC test, however, 18 raw milks of those samples responded positively to Charm II test. 2. By Lactek test, residual sulfamethazine was detected from 4 raw milks. Fifteen raw milks of 18 samples which were classified as positive one by Charm II test, showed positive response 3. Retention time of sulfonamides added at the level of 100ppb into sklm milk was ranged from 1.55 minute to 23.3 minute. Recovery rates of sulfonamides were variable from 6.7% upto 94.2% depended on the types of sulfonamlde. 4. Single type of sulfonamides was detected from 10 raw milk samples, 2 types of sulfonamides from 3 samples and 3 types from 2 raw milks by HPLC. 5. Sulfonamides was detected in this study were 5 types : 11 samples for sulfisomidine, 5 samples for sulfamethazine, 3 samples for sulfadlmethoxine, 2 samples for sulfathiazole and 1 sample for sulfadiazine. 6. The highest levels of residual sulfonamides was 210.3 ppb of sulfamethazine but the lowest concentration of residue was 2.2 ppb of sulfamethazine and sulfisomidine, respectively. Number of samples detected positively in this experiment were belows : above 100 ppb for 1 sample (4.5%) (sulfamethazine), 50~100 ppb for 4 samples (18.1%) (each 2 samples for sulfamethazine and sulfisomidine, respectively), 25~50 ppb for 6 samples (27.1%) (2 sulfisomidine, each 1 sample for sulfadiazine, sulfadimethoxine, sulfamethazine and sulfathiazole, respectively), 10~25ppb for 3 samples (13.7%) (3 sulfisomidine), and below 10ppb for 8 samples (36.4%) (4 sulfisomidine, 2 sulfadimethoxine and each 1 for sulfamethazine and sulfathiazole).

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Monitoring and Risk Assessment of Pesticide Residues for Circulated Agricultural Commodities in Korea-2013 (국내 유통 농산물의 잔류농약 모니터링 및 위해평가-2013년)

  • Kim, Jae-Young;Lee, Sang-Mok;Lee, Han-Jin;Chang, Moon-Ik;Kang, Nam-Sook;Kim, Nam-Sun;Kim, Heejung;Cho, Yoon-Jae;Jeong, Jiyoon;Kim, Mee Kyung;Rhee, Gyu-Seek
    • Journal of Applied Biological Chemistry
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    • v.57 no.3
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    • pp.235-242
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    • 2014
  • The purpose of this study is the establishment of scientific processes for making food safety policies. Thus, we investigated pesticide residue level of the agricultural commodities from market, and performed risk assessment. Fifteen agricultural items are chosen based on the frequency of Korean consumption. The samples were collected from 9 cities where populations are more than one million. Total 283 active ingredients were monitoring ( total sample number =232). Single-analysis of target pesticides was for three kinds of possible growth regulators and the multicomponent analysis was for 280 kinds of pesticides, a total of 283 species were selected to perform the pesticide residues. Before monitoring the analytes, the improvements of the analytical methods were done by method validations under the CODEX analytical method development guidelines and can produce metrics that represent the international standards applied in accordance with the guidelines. In addition to residual pesticides detected during monitoring we compare the ADI to EDI values using detected result and dietary consumption data which is extracted from annual market basket survey. The 163 samples were non-detected in the total 232 samples so it means that every agricultural commodity will residual pesticides-free in 70.3%. The detected residual pesticides showed for a total of 69 cases (29.7%). Two of samples violate Korean MRL (0.9%). The ratio of EDI compared to ADI resulted in only from 0.00087 to 0.902%. In result, we can assume that all detected residual pesticides are very safe level and current policies of Korean pesticides control may be working.