• Title/Summary/Keyword: LC/MS analysis

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Estimation of the Daily Human Intake of Acrylamide (AA) Based on Urinary N-acetyl-S-(2-carbamoylethyl)-cysteine (AAMA) and the Contribution of Dietary Habits in South Korean Adults (요중 AAMA에 의한 한국 성인 아크릴아마이드(AA)의 하루섭취량 추정 및 기여 식습관에 대한 분석)

  • LEE, Jin-Heon;LEE, Kee-Jae;KANG, Hee-Sook
    • Journal of Environmental Health Sciences
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    • v.42 no.4
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    • pp.235-245
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    • 2016
  • Objectives: This study estimated the adult Korean daily intake of acrylamide (AA) and investigated its relationship with demographic, lifestyle and dietary habits by using urinary concentrations of N-acetyl-S-(2-carbamoylethyl)-cysteine (AAMA). Methods: Human data (n=1870) was collected in a nationwide cross-sectional biomonitoring program representing the population (18-69 years) residing in South Korea. Urinary AAMA was analyzed with a LC-MS/MS system. Daily intakes of AA were estimated using mass daily AAMA, which was calculated through urinary AAMA concentration and daily creatinine excretion. Statistical analysis was performed with SAS procedures for calculating geometric means, confidence intervals and the exponentiated beta coefficient of multiple linear regressions. Results: Daily intake of AA was estimated at $0.475{\mu}g/kg$ body weight (BW) per day (95% confidence interval (CI): 0.447-0.503). In the case of current smokers, AA intake was $0.957{\mu}g/kg$ BW per day (95% CI: 0.847-1.067), which was significantly higher than that of former smokers and never smoked (p<0.0001). The strong affecting factors were age (95% CI: 0.68-1.14; p=0.0180), education level (95% CI: 1.05-1.42; p=0.0163), body mass index (BMI) (95% CI: 1.00-1.82; p<0.0001), and smoking status (95% CI: 0.97-3.05; p<0.0001). Korean dietary habits increasing AA intake were coffee (p=0.0005), cup noodles (p=0.0010) and canned foods (p=0.0005). Meanwhile, foods decreasing AA intake were fresh fruit (p=0.0076), cooked beef (p=0.0335) and cooked pork (p=0.0147). Conclusion: The Korean daily intake of AA in adults was estimated to be similar with those found in developed countries. The factors increasing daily AA intake were coffee, cup noodles and canned foods, and decreasing factors were fresh fruit, cooked beef and cooked pork.

Comparison of Chemical Constituents in Mung bean (Vigna radiata L.) Flour between Cultivation Regions and Seeding Dates

  • An, Yeon Ju;Kim, Mi Jung;Han, Sang Ik;Chi, Hee-Youn;Kwon, Chang;Kim, So Yeon;Yang, Yu Jin;Kim, Yun Ju;Moon, Hee Sung;Kim, Seung-Hyun;Chung, Ill-Min
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.65 no.4
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    • pp.457-467
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    • 2020
  • Legumes are one of the largest families of crop plants and are widely consumed and produced for their nutritional and commercial benefits. Mung bean (Vigna radiata L.) is a legume crop that contains various functional compounds ; moreover, it has strong antioxidant properties and is becoming an increasingly important food crop. However, most previous studies on mung beans have focused on their primary metabolites. In this study, we investigated the composition and contents of phenolic compounds, fatty acids, soyasapogenol and tocopherol in mung beans cultivated in different regions and cultivated at different seeding dates. Material analysis was conducted using the following methods: LC-MS/MS, GC-FID and HPLC-ELSD. In total, 57 different samples were analyzed. Thirteen phenolic compounds were detected in mung beans. Of these, vitexin and isovitexin were the most abundant compounds, accounting for approximately 99% of phenolic compounds. The difference in phenol compounds according to the seeding dates of mung bean was not statistically significant. The total fatty acid content in beans was the highest in Pyeongchang. Significant differences in total fatty acid content were found according to the cultivation regions. Crops grown in Sohyeon and Dahyeon showed the highest soyasapogenol B content in the Suwon region, and these were the lowest in Jeonju. The total tocopherol content of beans cultivated in Dahyeon and Sohyeon was the lowest and highest in Pyeongchang. Soyasapogenol B and total tocopherol content were not significantly different according to seeding dates. This study was conducted to obtain basic data for the cultivation of mung beans with a high content of various functional materials in terms of regional specialization and optimal seeding time.

Simultaneous Determination of Five Porphyrins in Human Urine and Plasma Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hur, Yeoun;Tae, Sookil;Koh, Yun-Joo;Hong, Sung-Hyun;Yoon, Young Ho;Jang, Haejong;Kim, Sooji;Kim, Kyeong Ho;Kang, Seung Woo;Lee, Youngshin;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.2
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    • pp.42-48
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    • 2014
  • A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed and validated for the simultaneous quantification of porphyrins (coproporphyrin, pentacarboxylporphyrin, hexacarboxylporphyrin, heptacarboxylporphyrin, and uroporphyrin) in human plasma and urine. Acidified plasma samples and urine samples were prepared by using liquid-liquid extraction using ethyl acetate and protein precipitation with acetonitrile, respectively. The separation was achieved onto a Synergi Fusion RP column ($150mm{\times}2.0mm$, $4{\mu}m$) with a gradient elution of mobile phase A (0.1% formic acid in 2 mmol/L ammonium acetate, v/v) and mobile phase B (20% methanol in acetonitrile, v/v) at a flow rate of $450{\mu}L$/min. Porphyrins and the internal standard (IS), coproporphyrin I-$^{15}N_4$, were detected by a tandem mass spectrometer equipped with an electrospray ion source operating in positive ion mode. Multiple reaction monitoring (MRM) transitions of the protonated precursor ions and the related product ions were optimized to increase selectivity and sensitivity. The proposed method was validated by assessing selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, and stability. The calibration curves were obtained in the range of 0.1-100 nmol/L and the LOQs were estimated as 0.1 nmol/L for all porphyrins. Results obtained from the validation study of porphyrins showed good accuracy, precision, recovery, and stability. Finally, the proposed method was successfully applied to clinical studies on the autism spectrum disorder (ASD) diagnosis of 203 Korean children.

Effect of Gongjindan, a Polyherbal Formula on the Pharmacokinetics Profiles of Sorafenib in Male SD Rats (1) - Single Oral Combination Treatment of Sorafenib 50mg/kg with Gongjindan 100mg/kg within 5min -

  • Kim, SeungMo;Lee, Chang Hyeong;Park, Soo Jin;Kang, Su Jin;Song, Chang Hyun;Han, Chang Hyun;Ku, Sae Kwang;Lee, Young Joon
    • Journal of Society of Preventive Korean Medicine
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    • v.18 no.2
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    • pp.89-100
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    • 2014
  • Objective : The co-administration effects of Gongjindan (GJD) on the pharmacokinetics (PK) of sorafenib were observed as a process of the comprehensive and integrative medicine. Methods : After sorafenib treatment, GJD was administered within 5 min. The plasma were collected at 30min before administration, 30min, 1, 2, 3, 4, 6, 8 and 24hrs after end of GJD treatment, and plasma concentrations of sorafenib were analyzed using LC-MS/MS methods. PK parameters of sorafenib ($T_{max}$, $C_{max}$, AUC, $t_{1/2}$ and $MRT_{inf}$) were analysis as compared with sorafenib single administered rats. Results : The absorption of sorafenib were significantly increased at 30min, 1, 6 and 6hrs after co-administration with GJD as compared with sorafenib single treated rats. Accordingly, the $AUC_{0-t}$ (47.20%) of sorafenib was significantly increased but $t_{1/2}$ (-30.63%) and $MRT_{inf}$ (-34.11%) in co-administered rats were non-significantly decreased. These findings are considered as direct evidences that GJD increased the oral bioavailability of sorafenib through increase of the absorption, when they co-administered within 5min. Conclusion : Based on the results, co-administration of GJD increased the oral bioavailability of sorafenib through increase of the gastrointestinal absorption. It is considered that the more detail pharmacokinetic studies should be tested to conclude the effects of GJD on the pharmacokinetics of sorafenib, when they were co-administered, like the effects after co-administration with reasonable intervals considering the $T_{max}$ of sorafenib (about 3.5hr-intervals) and after repeated co-administrations.Hence, concomitant uses of GJD with sorafenib may require close monitoring for potential drug interactions.

DEHP, DEP and DBP Exposure Analysis using Urinary Metabolites of Gyonggi Province University Students

  • Lee, JangWoo;Kho, YoungLim;Kim, SungKyoon;Choi, Kyungho;Hwang, SeongHee;Jeong, Jeeyeon;Kim, Pangyi
    • Journal of Environmental Health Sciences
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    • v.39 no.5
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    • pp.408-417
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    • 2013
  • Objectives: Phthalates are used as plasticizers in polyvinyl chloride (PVC) plastics. As phthalate plasticizers are not chemically bound to the PVC, they can leach, migrate or evaporate into indoor air and atmosphere, foodstuffs, other materials, etc. Therefore, humans are exposed through ingestion, inhalation, and dermal exposure over their entire lifetime, including during intrauterine development. In particular, university students have a great number of opportunities to contact products including phthalates during campus life (food packaging, body care products, cosmetic, lotions, aftershave, perfume etc.). The purpose of this study was to examine levels of phthalate exposure as undergraduate students begin to use pharmaceuticals and personal care products including phthalates. Methods: Phthalate metabolites, mono-ethyl phthalate (MEP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), mono-2- ethylhexyl phthalate (MEHP), {(mono-(2-ethyl-5-hydroxyhexyl) phthalate (MEHHP}, and mono-(2-ethlyl-5-oxohexyl) phthalate (MEOHP} were examined. 80 urine samples collected from university students were analyzed using LC/MS/MS(API 4000, Applied Bioscience) with on-line enrichment and columnswitching techniques. This study was carried out at Y university located in Gyonggi Province from 2008 to 2011. Results: The detection limit of phthalate metabolites were 0.03 ng/mL for MEP, 0.11 ng/mL for MnBP, 0.08 ng/mL for MiBP, 0.93 ng/mL for MEHP, 0.19 ng/mL for MEOHP and 0.16ng/mL for MEHHP. MnBP showed the highest urinary levels (median: 31.6 ug/L, 24.8 ug/g creatinine (cr)). Concentrations were also high for MEHHP (median: 24.1 ug/L, 19.0 ug/g cr), followed by MEOHP (median: 22.8 ug/L, 17.9 ug/g cr). In individual cases, the maximum level reached up to 348 ug/L, and 291 ug/g cr, respectively. The urinary and creatinine adjusted levels of MEP were lower than those for DBP and DEHP metabolites, but were higher in 95th percentiles. As a result, the mean daily DEP intake value was 2.3 ${\mu}g/kg$ bw/day, 3.5 ${\mu}g/kg$ bw/day for DEHP and 4.9 ${\mu}g/kg$ bw/day for DBP. Conclusion: These students' phthalate exposure levels were below the international safe level set by the EU, but higher than the 2012 KFDA survey of the age group from 3 to 18.

Effect of Jaeumkanghwatang (JEKHT), a Polyherbal Formula on the Pharmacokinetics Profiles of Tamoxifen in Male SD Rats (2) - Oral Combination Treatment of Tamoxifen 50 mg/kg with JEKHT 100 mg/kg on JEKHT 6-day Repeated Pretreated Rats with 8-day Repeated Co-administration -

  • Park, Soo Jin;Kwak, Min A;Park, Sung Hwan;Lee, Young Joon;Ku, Sae Kwang
    • Journal of Society of Preventive Korean Medicine
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    • v.20 no.2
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    • pp.97-109
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    • 2016
  • Objectives : The effects of Jaeumkanghwatang (JEKHT) co-administration on the pharmacokinetics of tamoxifen were observed after oral combination treatment of tamoxifen 50 mg/kg with JEKHT 100 mg/kg on JEKHT 6-day repeated oral pretreated rats with 8-day repeated co-administration to confirm the effects of JEKHT co-administration on the pharmacokinetics of tamoxifen. Methods : Six days after pretreatment of JEKHT 100 mg/kg, tamoxifen 50 mg/kg was co-administered with JEKHT 100 mg/kg, once a day for 8 days within 5 min. The blood were collected at 30 min before administration, 30 min, 1, 2, 3, 4, 6, 8 and 24 hrs after end of first and last 8th tamoxifen treatment, and plasma concentrations of tamoxifen were analyzed using LC-MS/MS methods. PK parameters of tamoxifen ($T_{max}$, $C_{max}$, AUC, $t_{1/2}$ and $MRT_{inf}$) were analysis as compared with tamoxifen single administered. Results : Six-day repeated oral pretreatment of JEKHT and 8-day repeated oral co-administration of tamoxifen within 5 min did not influenced on the plasma concentrations and pharmacokinetic parameters of tamoxifen, oral bioavailability, as compared with tamoxifen single treated rats, except for some negligible effects. Conclusions : It is concluded that JEKHT did not influenced on the plasma concentrations and pharmacokinetic parameters, the oral bioavailability of tamoxifen. Therefore, it is considered that co-administration of JEKHT and tamoxifen will be provide an effective novel treatment regimen on the comprehensive and integrative medicine for breast cancer patients, if they showed favorable synergic effects on the pharmacodynamics or reduce the tamoxifen treatment related toxicity and side effects in future studies.

Effect of Gamiondam-tang (GMODT), a Polyherbal Formula on the Pharmacokinetics Profiles of Tamoxifen in Male SD Rats

  • Ryu, Eun-A;Kang, Su-Jin;Song, Chang-Hyun;Lee, Bong-Hyo;Choi, Seong-Hun;Han, Chang-Hyun;Lee, Young-Joon;Ku, Sae-Kwang
    • The Journal of Korean Medicine
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    • v.38 no.2
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    • pp.61-72
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    • 2017
  • Objectives: The effects of Gamiondam-tang (GMODT) co-administration within 5min on the pharmacokinetics (PK) of tamoxifen were observed as a process of the comprehensive and integrative medicine, combination therapy of tamoxifen with GMODT to achieve synergic pharmacodynamics and reduce toxicity on the breast cancer. Methods: After 50mg/kg of tamoxifen treatment, GMODT 100mg/kg was administered within 5min. The plasma were collected at 30 min before administration, 30 min, 1, 2, 3, 4, 6, 8 and 24 hrs after end of GMODT treatment, and plasma concentrations of tamoxifen were analyzed using LC-MS/MS methods. PK parameters of tamoxifen (Tmax, Cmax, AUC, $t_{1/2}$ and $MRT_{inf}$) were analysis as compared with tamoxifen single administered rats using noncompartmental pharmacokinetics data analyzer programs. Results: Co-administration with GMODT induced increased trends of plasma tamoxifen concentrations to 1hr after end of administration, and then showed decreased trends of plasma tamoxifen concentrations, and especially significant (p<0.05) increases of plasma tamoxifen concentrations were demonstrated at 0.5hr after end of co-administration with GMODT and also related significant (p<0.05) decreases of $AUC_{0-inf}$ and $MRT_{inf}$ as compared with tamoxifen single formula treated rats, at dosage levels of tamoxifen 10 mg/kg and GMODT 100 mg/kg within 5 min, in this experiment. Conclusion: Based on the results of the present study, it is considered that single co-administration GMODT within 5min significantly inhibited the oral bioavailability of tamoxifen through variable influences on the absorption and excretion of tamoxifen, can be influenced on the toxicity or pharmacodynamic of tamoxifen.

Component Analysis and Anti-Proliferative Effects of Ethanol Extracts of Fruits, Leaves, and Stems from Elaeagnus umbellata in HepG2 Cells (보리수나무 열매, 잎 및 줄기 에탄올 추출물의 함유성분 분석과 간암 세포 증식억제 효과)

  • Kim, Min-Ju;Lim, Jong-Soon;Yang, Seun-Ah
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.6
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    • pp.828-834
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    • 2016
  • The aim of this study was to evaluate the physicochemical properties and antioxidant and anti-proliferative activities of different plant parts of Elaeagnus umbellata Thunb. extracted with ethanol (EtOH). EtOH extract of stems presenting the highest content of polyphenols showed the strongest 1,1-diphenyl-2-picrylhydrazyl radical scavenging activity ($EC_{50}=54.04{\mu}g/mL$). The total content of free amino acids decreased in the order of leaves (6,179.12 mg/100 g)> stems (1,211.69 mg/100 g)> fruits EtOH extract (378.88 mg/100 g), and asparagine (1,907.57 mg/100 g), ${\gamma}-aminobutyric$ acid (300.17 mg/100 g), and proline (233.48 mg/100 g) were the major free amino acid in leaves, stems, and fruits, respectively. Five phenolic compounds in each extract were measured by using liquid chromatography- tandem mass spectrometry, and gallic acid (98.95 mg/100 g) and (+)-catechin (1,575.99 mg/100 g) were present as major components in leaves and stems, respectively. EtOH extract of leaves showed the highest anti-proliferative activity against HepG2 cells as measured by 3-(4,5-dimethyl-thiazol-2-yl)-2,5-diphenyltetrazoliumbromide and lactate dehydrogenase assay but had no effects on Chang liver cells.

Application and Validation of an Optimal Analytical Method using QuEChERS for the determination of Tolpyralate in Agricultural Products (QuEChERS법을 활용한 농산물 중 제초제 Tolpyralate의 최적 분석법 선발 및 검증)

  • Lee, Han Sol;Park, Ji-Su;Lee, Su Jung;Shin, Hye-Sun;Kim, Ji-Young;Yun, Sang Soon;Jung, Yong-hyun;Oh, Jae-Ho
    • Korean Journal of Environmental Agriculture
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    • v.39 no.3
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    • pp.246-252
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    • 2020
  • BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R2≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.

Effect of Gamiondam-tang (GMODT), a Polyherbal Formula on the Pharmacokinetics Profiles of Tamoxifen in Male SD Rats (2) - Single Oral Combination Treatment of Tamoxifen 50 mg/kg with GMODT 100 mg/kg with 2.5 hr-intervals -

  • Ryu, Eun-A;Kang, Su-Jin;Song, Chang-Hyun;Lee, Bong-Hyo;Choi, Seong-Hun;Han, Chang-Hyun;Lee, Young-Joon;Ku, Sae-Kwang
    • Journal of Society of Preventive Korean Medicine
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    • v.21 no.2
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    • pp.127-137
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    • 2017
  • Objectives : In our previous study, single co-administration GMODT within 5 min significantly inhibited the oral bioavailability of tamoxifen through variable influences on the absorption and excretion of tamoxifen. Therefore, the object of this study was to elucidate the possible effects on the pharmacokinetics of tamoxifen after single oral co-administration of GMODT with 2.5 hr-intervals. Methods : After 50 mg/kg of tamoxifen treatment, GMODT 100 mg/kg was administered with 2.5 hr-intervals. The plasma were collected at 30 min before administration, 30 min, 1, 2, 3, 4, 6, 8 and 24 hrs after end of GMODT treatment, and plasma concentrations of tamoxifen were analyzed using LC-MS/MS methods. PK parameters of tamoxifen (Tmax, Cmax, AUC, $t_{1/2}$ and $MRT_{inf}$) were analysis as compared with tamoxifen single administered rats. Results : Two-half hr-interval co-administration with GMODT induced variable changes on the plasma tamoxifen concentrations as compared with tamoxifen single treated rats, and especially significant (p<0.05) increases of plasma tamoxifen concentrations were demonstrated at 0.5 (199.61%) and 1 hr (101.06%) after end of co-administration with GMODT, and also related significant (p<0.05) decreases of $t_{1/2}$ (-39.54%) and $MRT_{inf}$ (-43.94%) as compared with tamoxifen single formula treated rats, at dosage levels of tamoxifen 50 mg/kg and GMODT 100 mg/kg with 2.5 hr-intervals, in this experiment. Conclusions : According to the results, GMODT critically decreased on the oral bioavailability of tamoxifen through variable influences on the absorption and excretion of tamoxifen. Hence, the co-administration of GMODT and tamoxifen should be avoided in the comprehensive and integrative medicine, combination therapy of tamoxifen with GMODT on the breast cancer.