Citrinin determination in red fermented rice products by optimized extraction method coupled to liquid chromatography tandem mass spectrometry lc ms ms. Citrinin 3 rtrans4,6dihydro8hydroxy3,4,5trimethyl6oxo3h2benzopyran7carboxylic acid is a benzopyran derivative figure 2. Lcmsms determination of citrinin in traditional chinese. In the lc ms ms analysis of xuezhikang, it is supposed to be no peak detected at the retention time of citrinin. Cit can cooccur with ochratoxin a ota, a mycotoxin also known for its nephrotoxicity, and this raises concern regarding possible combined effects. Highly sensitive and rapid simultaneous method for 45 mycotoxins in baby food samples by hplc ms ms using fast polarity switching 6 extraction and ionisation recovery for aflatoxins was.
Homepagedin standards din en 17203 foodstuffs determination of citrinin in food by liquid chromatography tandem mass spectrometry lc ms ms sponsored link. A rapid and sensitive rphplc method with fluorescence detection at. Inclusion of the aflatoxins in this survey required additional method development. Coupled chromatography ms systems are popular in chemical analysis because the individual capabilities of each technique are enhanced synergistically. Assessment of bisphenol a specific migration from packaging. Lcmsms analysis of citrinin on ascentis express phenyl. High levels of citrinin may affect the liver in addition to the kidney. Citritest hplc is a quantitative method for detection of citrinin in kogi red rice and corn that uses monoclonal antibodybased affinity chromatography. Comparing to hplc, gc owns higher sensitivity and could be e. Predicted gc ms spectrum gc ms nonderivatized 70ev, positive. Evaluation of citrinin occurrence and cytotoxicity in. The samples are extracted with dichloromethane with the addition of phosphoric acid, and the extract is cleaned up on. Although all these methods can successfully determine mycotoxins, issues like false positive results, unfit for quantification of multicomponent mycotoxins, and the level of sensitivity still need to overcome.
The liquid chromatography tandem mass spectrometry lcmsms method for the citrinin cin determination in red rice was. An ideal cleanup step for any hplc, citritest hplc provides precise numerical results in parts per billion levels. The mycotoxin citrinin cit deserves attention due to its known toxic effects in mammalian species and a widespread occurrence in food commodities, often along with ochratoxin a, another nephrotoxic mycotoxin. A rapid and sensitive method was developed and validated for citrinin determination in red fermented rice products by liquid chromatography tandem mass spectrometry lcmsms under the selected reaction monitoring mode. Citrinin, a mycotoxin from penicillium citrinum, plays a role. In the past, various analytical methods of citrinin determination have been published. Development and validation of an lcmsms method for the. Citrinin by hplc and lcmsms trilogy analytical laboratory. The presence of citrinin in xuezhikang capsule has been a concern due to its ingredient which is derived from monascus fermented rice.
The lc handbook guide to lc columns and method development the lc handbook guide to lc columns and method development agilent crosslab combines the innovative laboratory services, software, and consumables competencies of agilent technologies and provides a direct connection to a global team of scientific and. The highest amount of afs was found in red chilli 219. The flow rates used in lc ms should be less than those used for hplc. Gcms was developed for the direct analysis of metabolites produced by several fusarium organisms without any chemical derivatization. The columns contain a gel suspension of monoclonal antibody specific to the toxins. Liquid chromatography mass spectrometry lc ms is fast becoming the preferred tool of liquid chromatographers. Development and validation of an lc ms ms method for the simultaneous determination of citrinin and. Retention, thermodynamics, selectivity, zone spreading, kinetics, and resolution torgny fornstedt, patrik forssen, and douglas westerlund liquid chromatography is a very important separation method used in practically all chemistry.
Hplc analysis of citrinin in red yeast rice article pdf available in food science and biotechnology 124. Pdf the liquid chromatography tandem mass spectrometry lcmsms method for the citrinin cin determination in red rice was developed. Api 4000 lc ms ms system hardware manual about this manual 7 glossary provides a list of api 4000 lc ms ms system and related mass spectrometry terminology used in this manual. A validated rphplc method for the determination of citrinin. Home products markets technology regulations safety data sheets certificates of analysis. Numerous and frequentlyupdated resource results are available from this search. Qualitative detection and quantitative detection of mycotoxins in spices were analyzed by elisa and further confirmed by lc ms ms. Hplc analysis of seven antiepileptic drugs and caffeine overlay of six consecutive runs on an agilent zorbax sbc18, 4.
Hplc analysis with fluorescence detection was used to determine citrinin levels. Highthroughput determination of citrinin in rice by ultra. Syringe filter selection for hplc or lc ms samples appropriate mixer volume for hplc and uhplc applications common causes of baseline noise in hplc, uhplc. Research article mycobiota and natural incidence of aflatoxins, ochratoxin a, and citrinin in indian spices confirmed by lc ms ms punamjeswalanddhirajkumar. Hplc application id no 15537 citrinin analysis using luna c182 column. A validated rphplc method for the determination of citrinin in. The analyses were conducted using hplcfld for ota, gcms for don.
Lc ms is a hyphenated technique, which combines the separating power of high performance liquid chromatography hplc, with the detection power of mass spectrometry. Citrinin determination in red fermented rice products by. Reliable information about the coronavirus covid19 is available from the world health organization current situation, international travel. Oclcs webjunction has pulled together information and resources to assist library staff as they consider how to handle coronavirus. Hplc, lc ms ms, citrinin, xuezhikang capsule, monascus introduction cintrinin, a toxic product of secondary metabolite of fungi, such as aspergillus, penicillium, and monascus species, is known to lead to serious health problems 1. Citrinin ctn is a hepatonephrotoxic mycotoxin produced by fungi genera of aspergillus, monauscus and penicillium. Simple and sensitive gcselected ion monitoring mass. As citrinin it is neutral but when it is excreted in the alkaline urine it becomes a phenol which is rapidly reabsorbed by the kidney where it tautomerizes back to citrinin. Request pdf highthroughput determination of citrinin in rice by ultrahighperformance liquid chromatography and fluorescence detection uhplcfl a rapid, simple and effective method for the.
This is to ensure complete ionization and to maintain the detection sensitivity of the ms. Analysis of cocoa products for ochratoxin a and aflatoxins. Standard foodstuffs determination of citrinin in food. Determination of citrinin in food by liquid chromatography tandem mass spectrometry lc ms ms maintenance will be taking place for bsi shop on saturday 28th march between 08. Citrinin was isolated in the 1930s and produced by penicillium citrinum. Bsi shop may be unavailable or may have limited functionality whilst this work is being carried out. Research article mycobiota and natural incidence of. Apr, 2020 lc ms involves separating mixtures in accordance with their physical and chemical properties, then identifying the components within each peak and detecting based on their mass spectrum. Imprinted solid phase extraction purification, hplc separation, and fluorescence detection michael appell, michael a. L of sample was injected into lc ms ms agilent containing the mobile phase of. In this study, a new quantitative method is described for the determination of five alternaria toxins and citrinin in tomato and tomato juice samples based on lc ms ms detection. Hplcms could exert its advantages for trace level detection and con.
Mycobiota and natural incidence of aflatoxins, ochratoxin. Alternaria toxins and citrinin are currently under consideration by the european commission. The fungal toxin citrinin is a major problem in many cereals and particularly in red yeast rice. It is a popular analytical technique used for the separation, identification and quantification of each constituent of mixture. The limit of detection lod value obtained was 1030 times lower using uhplc msms than hplcfl for aqueous simulants, whereas the limit of quantifi. Determination of citrinin in red yeast rice european commission. Development of a method for the determination of citrinin in. Apr 11, 2011 citrinin is a toxic product usually produced during the monascus fermentation. Most commonly, highperformance liquid chromatography hplc with diode array detection dad andor with mass spectrometry were reported for the determination of monacolins or monacolin k and citrinin. New method of citrinin determination by hplc after polyamide. Monitoring on the presence of phomopsins in lupinbased food and feed on the eu market. Liquid chromatography mass spectrometry lcms for citrinin was reported for the first. Cleanup of blood plasma by protein precipitation followed by lc ms ms based analysis allowed robust detection of.
This application note focuses on the hplc analysis of underivatized amino acids using ms detection. Report on the development of a method for the determination. Since red yeast rice is becoming more and more popular, the demand for methods for the analysis of citrinin increases. The objectives of this study were to validate a method to determine the specific migration of bpa in food simulants using both types of equipment. Hplc analysis of seven antiepileptic drugs and caffeine overlay of six consecutive runs on an. Apr 07, 20 eightyfive samples of cocoa products sampled in canada were analysed for ochratoxin a ota and aflatoxins in 20112012. Dp126 p126 immunoaffinity columns for use in conjunction with hplc or lcmsms. Immunoaffinity columns for use in conjunction with an hplc or lcmsms for detection of citrinin in a wide range of commodities. The lc ms ms chromatograms for the citrinin and xuezhikang are displayed in figure 3 and 4. Highly sensitive and rapid simultaneous method for 45.
Reversedphase hplc methods with either uv absorbance or fluorescence detection have also been applied. It is known as the yellowrice toxin discovered in japan. Citrinin is also produced by several aspergillus species including aspergillus terreus, aspergillus niveus, and aspergillus carneus. Methods using highperformance liquid chromatography with. Determination of citrinin using molecularly imprinted solid. Ms ms xiaofeng ji state key laboratory breeding base for zhejiang sustainable plant pest control, zhejiang academy of agricultural sciences, hangzhou, 310021 p. The procedure is based on monoclonal antibody technology, which makes the test highly specific, sensitive, rapid and simple to perform. Pdf methods for analysis of citrinin in human blood and. Liquid chromatography mass spectrometry lc ms is an analytical chemistry technique that combines the physical separation capabilities of liquid chromatography or hplc with the mass analysis capabilities of mass spectrometry ms. Gas chromatography and gc ms can be used to analyze a small percentage of the 9 million registered compounds. Pdf a new and sensitive method for determination of citrinin has been. Nuclear magnetic resonance has usually been used for confirmation of the structure in the presence of other mycotoxins. A methodology to determine patulin pat and citrinin cit in human urine and plasma using liquid chromatography coupled to tandem mass spectrometry was. Citrinin is synthesized by penicillium viridicatum and penicillium citrinum, and some species of aspergillus and monascus.
Development and validation of an lc ms ms method for the simultaneous determination of citrinin and ochratoxin a in a variety of feed and foodstuffs. Foodstuffs determination of citrinin in food by liquid chromatography tandem mass spectrometry lcmsms ssen 17203. Citrinin is a toxic product usually produced during the monascus fermentation. Standard foodstuffs determination of citrinin in food by. Citrinin in traditional chinese medicines was extracted by 70% methanol, and then purified by immunoaffinity columns. In this article, a hplc method for sensitive fluorescence detection, based on solid phase extraction in combination with a hplc gradient, is described. Mycotoxins are a group of natural contaminants in raw. Pdf hplc analysis of citrinin in red yeast rice researchgate.
High performance liquid chromatography with a mass detector hplcms was used for determining these compounds, the recovery amounts ranged from 86 to 108%, the values of the coefficients of variation were lower than 7% and the loq values varied from 4 to 100 g kg1. Simultaneous extraction and detection of ochratoxin a and. A method for the determination of the mycotoxin citrinin ct in rye, wheat and barley is described. The system consisted of a shimadzu lc 20at quaternary pump, rf10axl fluorescence detector, andacbm20acommunicationbusmodule.
Analysis of pharmaceutical substances using hplc and. Ctn contaminates grains, fruits, juices and vegetables cause various toxic effects to humans and animals. Various assays, including thinlayer chromatography tlc, enzymelinked immunosorbent assay elisa, and highperformance liquid chromatography hplc have been. To establish a sensitive and accurate method for the determination of citrinin in traditional chinese medicine by lc ms ms. A validated rphplc method for the determination of. Citrinin produces necrosis of the distal tubule epithelium in the kidney and is a ph dependent tautomer.
High performance liquid chromatography which is also known as high pressure liquid chromatography. The mass spectrometer was operated in the positive ionization electrosprayesi mode using multiple reaction monitoringmrm for. But, in contrast to ota, data on cit contamination in foods for human. A rapid and sensitive rp hplc method with fluorescence detection at. Mass spectrometry is a wideranging analytical technique, which involves the production and subsequent separation and identification of charged species. Determination of citrinin using molecularly imprinted solid phase extraction purification, hplc separation, and fluorescence detection analytes. Review on the qualitative and quantitative analysis of the. Foodstuffs determination of citrinin in food by liquid chromatography tandem mass spectrometry lc ms ms ssen 17203.
Effects of some flavonoids on the mycotoxin citrinin. Hplc and lcms frequently asked questions faq, training. Hplc is an advanced technique of column liquid chromatography. A rapid and sensitive method was developed and validated for citrinin determination in red fermented rice products by liquid chromatography tandem mass spectrometry lc. It is a powerful analytical technique that combines the resolving power of liquid chromatography with the detection specificity of mass. Penicillium citrinum produced citrinin in red chilli, black pepper, coriander, cumin, fenugreek, and dry ginger samples.
Preparation and characterization of monoclonal antibodies. Citrinin, a mycotoxin from penicillium citrinum, plays a role in inducing motility of paenibacillus polymyxa. Technical support ab sciex and its representatives maintain a staff of fullytrained service and technical specialists strategically located throughout the world. A practical guide to using and maintaining an lc ms system the combination of liquid chromatography lc and mass spectrometry ms has become the laboratory tool of choice for a broad range of industries that require the separation, analysis, and purification of mixtures of organic compounds. Determination of citrinin using molecularly imprinted. Guide to achieving reliable quantitative lcms measurements. Lc ms involves separating mixtures in accordance with their physical and chemical properties, then identifying the components within each peak and detecting based on their mass spectrum. The analysis of underivatized amino acids by hplc with ms. The commonly used analytical methods for ctn detection were tlc, hplc, lc ms ms, gc ms.
Citrinin was first recognized as a promising antibiotic but it was later found to cause kidney damage, retard growth, and eventually cause death in animals. Ctn in human and animal food and food products can be identified by several methods 5,8 and in human urine and plasma by liquid chromatography mass spectrometry. Because introduction liquid chromatography mass spectrometry lc ms is fast becoming the preferred. Bosma 2015 determination of citrinin using molecularly imprinted solid phase extraction. Maximum levels of these toxins in foods are currently under consideration by the european commission as a risk management measure. Liquid chromatography lc amino acids high performance liquid chromatography hplc mass spectrometry ms altus waters empower 3 chromatography data software cds created date. This document describes a procedure for the determination of the citrinin content in food cereals, red yeast rice ryr, herbs and food supplements by liquid chromatography tandem mass spectrometry lcmsms. Applications tn1119 page 2 of 8 for additional technical notes, visit. Human exposure, a key element in assessing risks related to these food contaminants, depends upon mycotoxin levels in food and on food consumption. However, in many applications it is necessary to isolate the target analyte from. Citrinin on 2 march 2012, the efsa panel on contaminants in the food chain contam adopted. Citrinin cit, produced by several penicillium, aspergillus, and monascus species, has been detected as contaminant in feeds, grains, and other food commodities. In this study a new method has been developed for the determination of five alternaria toxins and citrinin in wheat, tomato juice and sunflower seed samples based on a liquid chromatography tandem mass spectrometric lc ms ms method.
Citrinin has been determined by a number of methods, primarily thinlayer chromatography and highperformance liquid chromatography. During the method optimization different high performance liquid chromatography hplc columns packed with coreshell particles have been tested. Simultaneous analysis of alternaria toxins and citrinin in. Therefore, reducing the production of citrinin is of great interest. Methods for analysis of citrinin in human blood and urine. However, formatting rules can vary widely between applications and fields of interest or study. Jian yang, qi chen, weiping wang, jiajun hu, chuan hu. Hplc, lcmsms, citrinin, xuezhikang capsule, monascus. Citrinin determination in red fermented rice products by optimized extraction method coupled to liquid chromatography tandem mass spectrometry lc.
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