• Title/Summary/Keyword: tandem mass spectrometry #4

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Biotransformation of Panax ginseng extract by rat intestinal microflora: identification and quantification of metabolites using liquid chromatography-tandem mass spectrometry

  • Dong, Wei-Wei;Zhao, Jinhua;Zhong, Fei-Liang;Zhu, Wen-Jing;Jiang, Jun;Wu, Songquan;Yang, Deok-Chun;Li, Donghao;Quan, Lin-Hu
    • Journal of Ginseng Research
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    • v.41 no.4
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    • pp.540-547
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    • 2017
  • Background: In general, after Panax ginseng is administered orally, intestinal microbes play a crucial role in its degradation and metabolization process. Studies on the metabolism of P. ginseng by microflora are important for obtaining a better understanding of their biological effects. Methods: In vitro biotransformation of P. ginseng extract by rat intestinal microflora was investigated at $37^{\circ}C$ for 24 h, and the simultaneous determination of the metabolites and metabolic profile of P. ginseng saponins by rat intestinal microflora was achieved using LC-MS/MS. Results: A total of seven ginsenosides were detected in the P. ginseng extract, including ginsenosides Rg1, Re, Rf, Rb1, Rc, Rb2, and Rd. In the transformed P. ginseng samples, considerable amounts of deglycosylated metabolite compound K and Rh1 were detected. In addition, minimal amounts of deglycosylated metabolites (ginsenosides Rg2, F1, F2, Rg3, and protopanaxatriol-type ginsenosides) and untransformed ginsenosides Re, Rg1, and Rd were detected at 24 h. The results indicated that the primary metabolites are compound K and Rh1, and the protopanaxadiol-type ginsenosides were more easily metabolized than protopanaxatriol-type ginsenosides. Conclusion: This is the first report of the identification and quantification of the metabolism and metabolic profile of P. ginseng extract in rat intestinal microflora using LC-MS/MS. The current study provided new insights for studying the metabolism and active metabolites of P. ginseng.

Bioequivalence of Efexor® XR capsule to Venfaxine® OR tablet (Venlafaxine 75 mg) (이팩사® XR서방캅셀(벤라팍신, 75 mg)에 대한 벤팍신®OR서방정의 생물학적동등성)

  • Aryal, Dipendra Kumar;Oh, Soo-Yeon;Cho, Jong-Tae;Kim, Hyung-Gun;Kim, Yoon-Gyoon
    • Journal of Pharmaceutical Investigation
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    • v.37 no.6
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    • pp.397-402
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    • 2007
  • To evaluate the bioequivalence of two venlafaxine formulations, a standard 2-way randomized cross-over study was conducted in twenty-four healthy male Korean volunteers. A single oral dose of 75 mg of test formulation Venfaxine $OR^{(R)}$ (tablet) or reference formulation Efexor $XR^{(R)}$ (capsule) was administered with one-week washout period. Plasma concentrations of venlafaxine were assayed for over a period of 72 hours with a well validated method using liquid chromatography coupled to tandem mass spectrometry (LC-MS-MS). The $mean{\pm}S.D$. of maximum concentration $(C_{max})$ and elimination half-life $(t_{1/2})$ were $64.7{\pm}28.5$ ng/mL, $9.2{\pm}3.0$ h, and $67.2{\pm}30.2$ ng/mL, $9.9{\pm}3.5$ h for test and reference formulations, respectively. Time to reach maximum concentration $(T_{max})$ expressed in median value (range), for the test and the reference, were 10 h (6-14) and 8h (4-12), respectively. Similarly, area under the plasma concentration-time curve, from time zero to last sampling time $(AUC_t)$ and from time zero to time infinity $(AUC_{inf})$, for test and reference formulations were $1185{\pm}755$, $1326{\pm}896$ and $1124{\pm}737$, $1185{\pm}755$ $ng{\cdot}h/mL$, respectively. The parametric 90% confidence intervals on the mean of the differences between the two formulations (test-reference) of the log transformed values of $AUC_t$, and $C_{max}$ were 0.9630 to 1.1383 and 0.8650 to 1.0446, respectively. The overall results indicate that the two formulations are bioequivalent and can be prescribe interchangeably.

Residue analysis and risk assessment of ethoxyquin and ethoxyquin dimer in farmed fish (양식어류 중 Ethoxyquin과 Ethoxyquin dimer의 잔류분석 및 위해평가)

  • Choi, Young-Hee;Ko, Suk-Kyung;Ryu, Seung-Hee;Jin, Young-Hee;Kwak, Jae-Eun;Lee, Myung-Sook;Kim, Bog-Soon;Hang, In-Sook
    • Korean Journal of Food Science and Technology
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    • v.53 no.3
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    • pp.239-244
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    • 2021
  • In the present study, liquid chromatography tandem-mass spectrometry was used to conduct a risk assessment of ethoxyquin and ethoxyquin dimer residues in 288 farmed fish sold in wholesale and traditional markets in Seoul. The detection range (detection rate) of ethoxyquin and ethoxyquin dimer was 0.005~0.309 mg/kg (4.9%) and 0.001~2.828 mg/kg (69.8%), respectively. Ethoxyquin was detected only in freshwater eels, loaches, catfish, and flatfish, whereas ethoxyquin dimer was present in all fish species. To estimate the dietary exposure levels of ethoxyquin and ethoxyquin dimer, the hazard index, calculated using the acceptable daily intake and estimated daily intake, ranged from 0.001 to 0.300%. Our results indicate that there is no significant exposure risk to humans from these farmed fish despite 10 farmed fish samples exceeding the maximum residue level (1.0 mg/kg as the sum of ethoxyquin and ethoxyquin dimer).

Paralytic shellfish toxins (PSTs) and tetrodotoxin (TTX) of Korean pufferfish

  • Lee, Ka Jeong;Ha, Kwang Soo;Jung, Yeoun Joong;Mok, Jong Soo;Son, Kwang Tae;Lee, Hee Chung;Kim, Ji Hoe
    • Fisheries and Aquatic Sciences
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    • v.24 no.11
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    • pp.360-369
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    • 2021
  • Paralytic shellfish toxins (PSTs) and tetrodotoxin (TTX) are neurotoxins that display pharmacological activity that is similar to that of specific sodium channel blockers; they are the principle toxins involved in shellfish and puffer fish poisoning. In Korea, puffer fish is a very popular seafood, and several cases of accidental poisoning by TTX have been reported. Therefore, it is necessary to determine whether puffer fish poisoning incidents are caused by PSTs or by TTX. In this study, we used mouse bioassay (MBA) and liquid chromatograph-tandem mass spectrometry (LC-MS/MS) to determine the presence of PSTs and TTX in puffer fish from an area near Mireuk-do, Tong-Yeong on the southern coast of Korea from January through March, 2014. The toxicity of PSTs and TTX extracts prepared from three organs of each specimen was analyzed by MBA. Most of the extracts killed mice with typical signs of TTX and PSTs. The LC-MS/MS analysis of seven specimens of Takifugu pardalis and Takifugu niphobles, each divided into muscles, intestines, and liver, were examined for TTX. In T. pardalis, the TTX levels were within the range of 1.3-1.6 ㎍/g in the muscles, 18.8-49.8 ㎍/g in the intestines, and 23.3-96.8 ㎍/g in the liver. In T. niphobles, the TTX levels were within the range of 2.0-4.5 ㎍/g in the muscles, 23.9-71.5 ㎍/g in the intestines, and 28.1-114.8 ㎍/g in the liver. Additionally, the toxicity profile of the detected PSTs revealed that dcGTX3 was the major component in T. pardalis and T. niphobles. When PSTs were calculated as saxitoxin equivalents the levels were all less than 0.5 ㎍/g, which is below the permitted maximum standard of 0.8 ㎍/g. These findings indicate that the toxicity of T. pardalis and T. niphobles from the southern coast of Korea is due mainly to TTX and that PSTs do not exert an effect.

Development and Validation of an Analytical Method for β-Agonists in Livestock and Fishery Products Using LC-MS/MS (LC-MS/MS를 이용한 축·수산물 중 β-agonist계 시험법 개발 및 검증)

  • Lee, Tae Ho;Kim, Yu Ra;Park, Su Jeong;Kim, Ji Young;Choi, Jang Duck;Moon, Gui Im
    • Korean Journal of Environmental Agriculture
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    • v.41 no.2
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    • pp.135-151
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    • 2022
  • BACKGROUND: The β-agonists known as phenyl ethanolamine derivatives have a conjugated aromatic ring with amino group. They are used as tocolytic agents and bronchodilator to human and animal generally, and some of them are used as growth promoters to livestock. METHODS AND RESULTS: β-agonists in samples were extracted by 0.4 N perchloric acid and ethyl acetate. The target compounds were analyzed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS). Validation of method was performed according to CODEX guidelines (CAC/GL-71). The matrix matched calibration gave correlation coefficients>0.98, and the obtained recoveries were in the range of 62.0-109.8%, with relative standard deviation ≤ 20.1%. In addition, a survey was performed to inspect any residual β-agonist from 100 samples of livestock and fishery products and ractopamine was detected in one of the 100 samples. CONCLUSION(S): In this study, we established the analytical method for β-agonists through using the expanded target compounds and samples. And we anticipate that the established method would be used for analysis to determine veterinary drug residues in livestock and fishery products.

Investigation of Acrylamide Contents in Frozen Foods According to the Cooking Method (가열조리에 따른 냉동식품의 아크릴아마이드 함량조사)

  • You-Jin Lee;Myung-Gil Kim;Hye-Jung Kwon;Ho-Jeong Bae;Kyong-Suk Lim;Eun-Jin Baek;Myung-Jin Lee
    • Journal of Food Hygiene and Safety
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    • v.38 no.6
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    • pp.476-482
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    • 2023
  • This study aimed to investigate the acrylamide content in frozen food products after cooking. Twenty samples of bread (Group 1) and 30 samples of processed tuberous and corn vegetable products (Group 2) were selected. Acrylamide levels were quantified using liquid chromatography tandem-mass spectrometry (LC-MS/MS). The frozen food samples were heated using the air fryer cooking method according to the product packaging and were compared to ready-to-eat French fries (Group 3). The results showed that the acrylamide content was the highest in group 3, followed by that in group 2 and group 1. The acrylamide content of all the samples was found to be within the domestic recommended standard of 1 mg/kg. However, when the samples that exceeded EU benchmark level (0.5 mg/kg) were selected and cooked using the deep-fat frying method according to the product packaging, one of them showed the acrylamide content of 1.83 mg/kg, which exceeded the domestic recommended standard. The present study highlights the need for continued evaluation and management to reduce acrylamide contents in frozen foods, as increasing domestic exposure to acrylamide is concerning.

Case Report on NTBC Treatment of Type 1 Tyrosinemia Diagnosed through Newborn Screening (신생아 선별검사를 통해 진단된 1형 타이로신혈증의 NTBC 치료 사례 보고)

  • Ji Eun Jeong;Hwa Young Kim;Jung Min Ko
    • Journal of The Korean Society of Inherited Metabolic disease
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    • v.23 no.2
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    • pp.39-44
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    • 2023
  • Hereditary tyrosinemia type 1 (HT-1) is a metabolic disorder caused by biallelic pathogenic variants in the fumarylacetoacetate hydrolase (FAH) gene, which impairs the function of the FAH enzyme, resulting in the accumulation of tyrosine's toxic metabolites in hepatocytes and renal tubular cells. As a consequence, individuals with HT-1 exhibit symptomatic manifestations. Rapid diagnosis and treatment of HT-1 can prevent short-term death and long-term complications. A 15-day-old boy presented to the outpatient department with elevated levels of tyrosine on his newborn screening tests conducted at the age of 3 and 10 days, respectively. Further blood tests revealed increased levels of alpha-fetoprotein and amino acids including tyrosine and threonine. Urine organic acid tests indicated a significant elevation in tyrosine metabolites, as well as the presence of succinylacetone (SA), which led to the diagnosis of HT-1. Two pathogenic and likely pathogenic variants of FAH compatible with HT-1 were also detected. He began a tyrosine-restricted diet at one month old and received nitisinone (NTBC) at two months old. With continued treatment, the patient's initially elevated AFP level, detection of SA in the urine, and mild hepatomegaly showed improvement. During four years and seven months of treatment, there were no exceptional complications apart from an increase in tyrosine levels and a delay in speech. We report a case of tyrosinemia type 1 detected through newborn screening, treated with dietary restriction and NTBC, with a good prognosis.

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Analysis of dutasteride in human serum by LC-MS/MS (LC-MS/MS를 이용한 혈청 중 dutasteride 분석)

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Jung, Ki-Kyung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.76-82
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    • 2012
  • The determination and confirmation of dutasteride in human serum was performed by a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Beclomethasone as an internal standard (I.S.) was added to the serum and the mixed sample was pretreated by liquid-liquid extraction (LLE) with methyl tert-butyl ether (MTBE). The mass transitions of dutasteride and I.S. monitored in multiple reaction monitoring (MRM) were m/z 529.6${\rightarrow}$461.5 and m/z 409.3${\rightarrow}$391.2, respectively, and the retention times were 6.45 and 5.46 min, respectively. The calibration curve was linear in the concentration range of 0.5~30.0 ng/mL ($R^2$= 0.9999) and the limit of quantitation (LOQ) was found to be 0.5 ng/mL. The recovery of dutasteride was shown to be 66~72%. The intra-day assay precision and accuracy were in the range 3.5~5.5% and 85.7~89.9%, respectively, and the interday assay precision and accuracy were in the range 4.2~5.8% and 90.8~95.8%, respectively.

Optimization of Analytical Methods for Octacosanol in Related Health-functional Foods with GC-MS (GC-MS를 이용한 건강기능식품 중 옥타코사놀 분석법 개발 연구)

  • Lee, Jin Hee;Oh, Mi Hyune;Lee, Kyung Jin;Kim, Yang Sun;Keum, Eun Hee;Park, Ji Eun;Cho, Mee Hyun;Seong, Min Hye;Kim, Sang A;Kim, Mee hye
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.266-271
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    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

Method Development for Determination of Multi-Mycotoxins in Chicken Liver and Kidney Tissues by LC-MS/MS (LC-MS/MS를 이용한 닭 간과 신장 중 곰팡이 독소 6종 동시분석법 개발)

  • Kim, Soohee;Kim, Kwang-Nam;Kim, Hyobi;Song, Jae-Young;Park, Sung-Won
    • Korean Journal of Poultry Science
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    • v.43 no.2
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    • pp.111-118
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    • 2016
  • Mycotoxins are secondary metabolites produced by molds, such as Aspergillus, Fusarium and Penicillium, that have adverse effects on animals and humans. Aflatoxin, ochratoxin, zearalenone, fumonisin and deoxynivalenol are the mycotoxins of greatest agro-economic importance and cause acute disease called mycotoxicoses. Mycotoxicosis in poultry birds results in decreased meat/egg production, immunosuppressant, and hepatotoxicosis. Some of toxins or their metabolites may be retained in animal or human tissues and induce health problems. This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous detection and quantification of mycotoxins, such as aflatoxin $B_1$, aflatoxin $M_1$, ochratoxin A, zearalenone, fumonisin B and deoxynivalenol, in chicken liver and kidney tissues. The mycotoxins were extracted and purified using modified QUECHERS methods, separated by LC and detected by an electrospray ionisation interface (ESI) and tandem MS. Good precision and linearity were observed for most of six mycotoxins. The recovery test for each mycotoxin in liver and kidney tissues mostly indicated good average recovery rates between 80.94% and 98.10% and the coefficient of variation mostly under 13.78%, except for aflatoxin $M_1$ and fumonisin $B_1$. The limit of detection (LOD) for six mycotoxins was $7.6{\sim}145.79{\mu}g/kg$ in liver tissues and $6.07{\sim}197.20{\mu}g/kg$ in kidney tissues. The quantification limits (LOQ) for 6 mycotoxins were in the range $23.04{\sim}441.78{\mu}g/kg$ in liver tissues and $18.40{\sim}597.59{\mu}g/kg$ in kidney tissues, respectively. The developed multi-mycotoxin method in this study permits simultaneous, simple, and rapid determination of several co-existing mycotoxins in chicken liver and kidney tissues.