1、红曲菌两种新的荧光代谢产物的研究 2、脱氧雪腐镰刀菌烯醇胶体金免疫层析试纸条的研制
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摘要
红曲在我国古代也称“丹曲”,传统的红曲是指以大米为原料,接种红曲菌经固体发酵而成的红曲米。红曲在中医上具有健脾化食、燥湿化痰、活血化瘀等功效;工业上常用于制作红曲米酒和腌渍肉、鱼等。红曲中含有多种代谢产物,例如醇类物质、酶类物质、有机酸、红曲色素、莫纳可林K(Monacolin K,MK)、γ-氨基丁酸(GABA)等。其中大部分代谢产物具有降血压、降血脂、抗菌、抗氧化和抗癌等重要的生理活性。红曲菌发酵代谢产物成分复杂,虽然已有较多代谢产物被分离和鉴定,如红曲色素、MK、桔霉素等,但有关红曲中荧光物质的报道甚少。
本论文的第一部分分离和鉴定了红曲中两种新的荧光物质,并对其部分性质进行了研究。主要研究及结果如下:
1采用硅胶柱层析和半制备型HPLC首次分离、纯化得到了红曲中两种新的荧光物质。两者的紫外吸收光谱相似,分子量分别为356和384,命名为monasfluore A(MFA)和monasfluore B(MFB)。分别对MFA和MFB进行荧光光谱扫描,确定了两者的最佳激发波长和发射波长分别为λex=396 nm和λem=460 nm。采用UV、HPLC、LC-MS、LC-MS/MS、HRMS和NMR等手段对MFA和MFB的结构进行了表征。结果发现MFA为MFB类似物,两者的基本骨架完全相同,具有相同的多聚酮发色团结构,两者之间分子量相差28,只是侧链相差两个亚甲基,MFA含有6个碳原子的己基侧链,而MFB含有8个碳原子的辛基侧链。这与已知结构的6种红曲色素相类似,也属于Azaphilones类代谢产物。
2首次建立了用HPLC同时测定红曲样品中MFA和MFB的方法。采用色谱柱Symmetry C_(18)(5μm,250×4.6 mm I.D.)和乙腈-水(77:23,v/v)流动相作为分离条件;λex=396 nm,λem=460 nm作为荧光检测器的检测波长,以自制的MFA和MFB为对照品进行定量分析。其中MFA的线性方程为Y=772.5X-289.2,相关系数R=0.9994,线性范围为0.5-10 ng/mL,平均回收率为85.2%,相对标准偏差为4.2%;MFB的线性方程为Y=2376.6X+1346.4,相关系数R=0.9972,线性范围为0.25-5 ng/mL,MFB的平均回收率为82.3%,相对标准偏差为5.3%。多次测定的相对标准偏差均小于3%,具有较好的重复性和稳定性。采用建立的HPLC方法检测了经20株红曲菌发酵的大米,结果发现不同红曲菌株发酵的大米中,MFA和MFB的含量不一,其中含量最高的为13号菌,MFA和MFB的含量分别为81.4 g/kg和26.3 g/kg,而14号菌发酵的大米中的MFA和MFB含量最低,分别为0.01 g/kg和0.003 g/kg。
3首次对MFA和MFB的强酸和强碱、热稳定性、光稳定性和与BSA相互作用进行了研究。结果发现,MFA和MFB的热稳定性和光稳定性差,在酸性条件下比碱性条件稳定。与MFA相比,MFB与BSA的作用力明显增强,可能是由于MFB含有更长的侧链,具有更强的亲脂性,与BSA之间的疏水作用更强。
4采用MTT法首次研究了MFA和MFB对人肺癌细胞(A549)、人肝癌细胞(HepG2)和人二倍体细胞(WI-38)增殖的抑制作用,结果发现MFA和MFB对A549和HepG2细胞有较明显的抑制作用,而对WI-38细胞抑制相对较弱。MFA和MFB对HepG2细胞抑制的IC_(50)值分别为12.4和7.1μg/mL;MFA和MFB对A549细胞抑制IC_(50)值分别为16.3和10.6μg/mL。MFB对细胞抑制的作用明显强于MFA,提示可能与两者的侧链长度不同有关。
脱氧雪腐镰刀菌烯醇(Deoxynivalenol,DON)是一种常见的真菌毒素,广泛存在于小麦和玉米等谷物及其制品中,对人类和动物构成很大的威胁。目前,有关DON的检测方法主要有薄层层析法、气相色谱法(采用电子捕获检测器或质谱检测)、液相色谱法(采用紫外、荧光、质谱或质谱-质谱检测)和ELISA等。上述方法不仅检测设备昂贵、样品前处理复杂、耗时费力,而且需要专业人员操作,难于在基层普及和推广,更不适合现场和野外大规模的快速检测。
本研究第二部分研制了谷物及其制品中DON的胶体金免疫层析快速检测试纸条。该试纸条准确灵敏、特异性好、操作简单、快速,无需昂贵的设备,适合于现场和批量样品的检测分析。主要研究及结果如下:
1对金标抗体的制备的主要影响因素进行了研究。采用ELISA测定标记的金标抗体离心后的上清液与参照液中抗体含量,确定了胶体金最佳标记pH值为7.0;采用盐析滴定法确定了制备金标抗体最适标记抗体量为30μg/mL。
2优化了试纸条的工艺条件。选用P40膜作为层析膜;金标抗体的稀释度为1:3(即稀释3倍);P40膜上喷有浓度分别为800μg/mL和1 mg/mL的检测抗原(DON-CBSA)和羊抗鼠IgG二抗,喷量均为0.74μL/cm;在上样液中加上0.005%的阴离子表面活性剂,能很好的消除试纸条上金标抗体与检测抗原之间由于静电作用而产生的非特异性吸附。
3该试纸条的灵敏度较高,为50 ng/mL;特异性较好,该试纸条与黄曲霉毒素B_1、玉米赤霉烯酮、赭曲霉毒素A、T-2毒素、HT-2毒素和桔霉素未见有交叉反应;稳定性较好,25℃至少可保存5-6个月。
4对样品前处理进行了研究。结果发现,在本实验中样品颗粒大小、不同水质、搅拌时间和不同静置时间等对试纸条的检测结果无明显影响。考虑到现场快速检测情况,称取粉碎1-2 min后的样品5 g,加入100 mL纯净水或自来水提取,用玻璃棒剧烈搅拌2 min,静置2 min,进行检测,10 min后判读结果,整个过程只需15 min。
5采用自制的DON快速检测试纸条和Ridascreen Fast ELISA试剂盒分别检测了市售的小麦和玉米样品,对检测结果进行比较和分析,实验显示,两种方法的检测结果一致。
Red yeast rice is produced by growing Monascus sp.on rice to produce a red-colored product.Although for years it has been known that there are six pigments and other metabolic products from Monascus sp.,such as alcohols,organic acids,and substances with a wide range of biological and therapeutic benefits,including anticarcinogenic,antioxidative,and hypolipidemic activities,which have been described,in the past decade,some new pigments and metabolites have been isolated and their chemical structures have been characterized. However,some fluorescent compound products from Monascus sp.have received less attention.Therefore,the first part in this study,two new Monascus metabolites from red yeast rice were studied.
1 Two new Monascus metabolites with similar fluorescence spectra(λex=396 nm,λem=460 nm) and UV absorption spectra were detected.They were isolated by rechromatography on a silica gel column and semipreparative HPLC,and two strong blue fluorescent compounds were obtained.Their structures were elucidated by electrospray ionization mass spectrometry(ESI-MS),electrospray ionization tandem mass spectrometry(ESI-MS/MS), intensive ESI-MS,and nuclear magnetic resonance spectroscopy(1H NMR,13C NMR,COSY, and HMBC) studies.High-resolution mass spectrometry indicated the molecular formulas C_(21)H_(24)O_5 and C_(23)H_(28)O_5.The two new compounds,named monasfluore A(MFA) and monasfluore B(MFB),respectively,contain a alkyl side chain,γ-lactone,and propenyl group, whereas themore lipophilic compound,MFB,is a higher homologue of MFA,with the more lipophilic octanoyl instead of the hexanoyl side chain.
2 A specific HPLC method has been developed and validated for the simultaneous determination of MFA and MFB in red yeast rice.Chromatographic separation was achieved at room temperature using a 250×4.6 mm I.D.,5μm Symmetry C_(18) column(Waters),with isocratic elution of water/acetonitrile(23:77,v/v) at a flow rate of 0.8 mL/min.The average recoveries of the method for MFA and MFB were 85.2%and 82.3%,respectively,and the RSD were 4.2%and 5.3%,respectively.The linear equations of MFA and MFB were Y=772.5X-289.2 and Y=2376.6X+1346.4 respectively,and the correlation coefficients were 0.9994 and 0.9972,respectively.The linear ranges of MFA and MFB were from 0.5 to 10 ng/mL and from 0.25 to 5 ng/mL,respectively.20 samples of red yeast rice were analyzed directly by this method.The results showed that the maximum production of MFA and MFB by NO.13 Monascus sp.were 81.4 and 26.3 g/kg,respectively,and the minimum production of MFA and MFB by NO.14 Monascus sp.were 0.01 and 0.003 g/kg,respectively.
3 The stabilties of MFA and MFB for strong acid,strong alkali,heat and light were studied, and the interaction between BSA and MFA and MFB were also studied.The results showed that the stabilties of MFA and MFB for alkali,heat,light were poor,but the stabilties of MFA and MFB for strong acid were better than for strong alkali.MFA is a lower homologue of MFB,with the less lipophilic hexanoyl instead of octanoyl side chain,and this results in a less interaction with BSA.
4 The inhibition proliferation of cancer cell lines,Hep G2 and A549,and human normal cell lines,WI-38,were determined by methyl thiazolyl tetrazolium(MTT) assay method.The results indicate that the notable inhibition proliferation on A549 and Hep G2 are found in MFA and MFB,but without too significant inhibition toward normal fibroblasts WI-38 at the same concentrations of 5-20μg/mL.The concentrations of 50%percent inhibition(IC_(50)) of MFA in the two tumor cell lines(HepG2 and A549),were found to be around 12.4 and 16.3μg/mL, respectively,and IC_(50) of MFB in HepG2 and A549 were about 7.1 and 10.6μg/mL These results indicate that the length of the saturated side chain on the ketonic carbonyl group of MFB is an important factor toward the inhibition proliferation.
Deoxynivalenol(DON) is produced largely by Fusarium fungi,which are widespread in nature and commonly contaminate many cereal grains such as wheat,corn,barley,oats,and rye intended for human and animal consumption.At present,the determination of DON is normally carried out using gas chromatography(GC) with either electron capture or mass spectrometric(MS) detection,or high-performance liquid chromatography(HPLC) with ultraviolet(UV) detection,fluorescence detection after postcolumn derivatization or MS detection.The merit of chromatographic methods is that they allow highly sensitive measurements of individual toxins simultaneously.But they are thought to be unsuitable for measuring many samples within a short time,because lengthy sample preparation such as column cleanup and derivation is required to achieve high sensitivity.Furthermore, high-priced measurement machines and highly qualified personnel are required in order to apply these methods,and the running costs are generally high.In addition,some researchers have established enzyme-linked immunosorbent assay(ELISA) for DON,and it is also unsuitable for on-site detection because it requires labor-intensive operations including incubation,washing,and enzymatic reactions during signal generation.
There is a need for rapid and cheap but reliable methods that can be conducted and interpreted by users who are close to the site of contamination.Therefore,the second part in this study,a colloidal gold immunochromatographic strip(ICS) test for rapid detection of DON in wheat and maize samples was developed.
1 For the development of a sensitive ICS test,it is necessary for the optimal pH and amount of antibody for the labeled gold colloid.After centrifugation,the titer of supernatant and original antibody was compared by ELISA to determine the optimal pH value.The minimum amount of anti-DON Mab was determined by adding NaCl to colloidal gold particles containing different amounts of Mab.After reaction with NaCl,a colloidal gold solution containing minimum Mab could be kept reddish or red-orange color.It was found that the optimal pH value for the labeled colloidal gold was 7.0 and the minimum amount of Mab was 30μg for 1 mL colloidal gold.
2 A total of 0.74μL per 1 cm of DON-cationic bovine serum albumin(CBSA)(0.8 mg/mL) conjugate and goat anti-mouse IgG antibody(1.0 mg/mL) were sprayed onto NC membrane(P 40) as the T and C line,and a total of 5μL/cm of colloidal gold-labelled anti-DON Mab diluted three times,was jetted on the treated conjugate pad.In addition,the nonspecific reaction was removed by adding 0.005%anion surfactant to the solution,and it appears that anion surfactant may neutralize the positive charge of the CBSA.
3 The cross-reacted rates between the DON rapid test strip and aflatoxin B1 nivalenol,T-2, HT-2,ZEN,and citrinin were poorly.The ICS test had a visual detection limit of 50 ng/mL for DON.The validity of DON rapid test strip was at least 5-6 months at 25℃.
4 The sample preparation methods for the ICS were investigated.It was found that the test results of ICS were not significantly affected by size of the sample,different water,mixing time and standing time in this experminement.To perform the test,5 g of sample was extracted in a ratio of 1:20 with water by shaking for 2 min,standing 2 min,and then the extract directly test without further cleanup steps.After 10 min,the test results were obtained, and the whole process was about 15 min.
5 Analysis of DON in wheat and maize samples revealed that data obtained from ICS test were in a good agreement with those obtained from ELISA.The results demonstrate that the ICS test can be used as a reliable,rapid,cost-effective and convenient qualitative tool for on-site screening technique of DON in wheat and maize samples.
本论文的第一部分分离和鉴定了红曲中两种新的荧光物质,并对其部分性质进行了研究。主要研究及结果如下:
1采用硅胶柱层析和半制备型HPLC首次分离、纯化得到了红曲中两种新的荧光物质。两者的紫外吸收光谱相似,分子量分别为356和384,命名为monasfluore A(MFA)和monasfluore B(MFB)。分别对MFA和MFB进行荧光光谱扫描,确定了两者的最佳激发波长和发射波长分别为λex=396 nm和λem=460 nm。采用UV、HPLC、LC-MS、LC-MS/MS、HRMS和NMR等手段对MFA和MFB的结构进行了表征。结果发现MFA为MFB类似物,两者的基本骨架完全相同,具有相同的多聚酮发色团结构,两者之间分子量相差28,只是侧链相差两个亚甲基,MFA含有6个碳原子的己基侧链,而MFB含有8个碳原子的辛基侧链。这与已知结构的6种红曲色素相类似,也属于Azaphilones类代谢产物。
2首次建立了用HPLC同时测定红曲样品中MFA和MFB的方法。采用色谱柱Symmetry C_(18)(5μm,250×4.6 mm I.D.)和乙腈-水(77:23,v/v)流动相作为分离条件;λex=396 nm,λem=460 nm作为荧光检测器的检测波长,以自制的MFA和MFB为对照品进行定量分析。其中MFA的线性方程为Y=772.5X-289.2,相关系数R=0.9994,线性范围为0.5-10 ng/mL,平均回收率为85.2%,相对标准偏差为4.2%;MFB的线性方程为Y=2376.6X+1346.4,相关系数R=0.9972,线性范围为0.25-5 ng/mL,MFB的平均回收率为82.3%,相对标准偏差为5.3%。多次测定的相对标准偏差均小于3%,具有较好的重复性和稳定性。采用建立的HPLC方法检测了经20株红曲菌发酵的大米,结果发现不同红曲菌株发酵的大米中,MFA和MFB的含量不一,其中含量最高的为13号菌,MFA和MFB的含量分别为81.4 g/kg和26.3 g/kg,而14号菌发酵的大米中的MFA和MFB含量最低,分别为0.01 g/kg和0.003 g/kg。
3首次对MFA和MFB的强酸和强碱、热稳定性、光稳定性和与BSA相互作用进行了研究。结果发现,MFA和MFB的热稳定性和光稳定性差,在酸性条件下比碱性条件稳定。与MFA相比,MFB与BSA的作用力明显增强,可能是由于MFB含有更长的侧链,具有更强的亲脂性,与BSA之间的疏水作用更强。
4采用MTT法首次研究了MFA和MFB对人肺癌细胞(A549)、人肝癌细胞(HepG2)和人二倍体细胞(WI-38)增殖的抑制作用,结果发现MFA和MFB对A549和HepG2细胞有较明显的抑制作用,而对WI-38细胞抑制相对较弱。MFA和MFB对HepG2细胞抑制的IC_(50)值分别为12.4和7.1μg/mL;MFA和MFB对A549细胞抑制IC_(50)值分别为16.3和10.6μg/mL。MFB对细胞抑制的作用明显强于MFA,提示可能与两者的侧链长度不同有关。
脱氧雪腐镰刀菌烯醇(Deoxynivalenol,DON)是一种常见的真菌毒素,广泛存在于小麦和玉米等谷物及其制品中,对人类和动物构成很大的威胁。目前,有关DON的检测方法主要有薄层层析法、气相色谱法(采用电子捕获检测器或质谱检测)、液相色谱法(采用紫外、荧光、质谱或质谱-质谱检测)和ELISA等。上述方法不仅检测设备昂贵、样品前处理复杂、耗时费力,而且需要专业人员操作,难于在基层普及和推广,更不适合现场和野外大规模的快速检测。
本研究第二部分研制了谷物及其制品中DON的胶体金免疫层析快速检测试纸条。该试纸条准确灵敏、特异性好、操作简单、快速,无需昂贵的设备,适合于现场和批量样品的检测分析。主要研究及结果如下:
1对金标抗体的制备的主要影响因素进行了研究。采用ELISA测定标记的金标抗体离心后的上清液与参照液中抗体含量,确定了胶体金最佳标记pH值为7.0;采用盐析滴定法确定了制备金标抗体最适标记抗体量为30μg/mL。
2优化了试纸条的工艺条件。选用P40膜作为层析膜;金标抗体的稀释度为1:3(即稀释3倍);P40膜上喷有浓度分别为800μg/mL和1 mg/mL的检测抗原(DON-CBSA)和羊抗鼠IgG二抗,喷量均为0.74μL/cm;在上样液中加上0.005%的阴离子表面活性剂,能很好的消除试纸条上金标抗体与检测抗原之间由于静电作用而产生的非特异性吸附。
3该试纸条的灵敏度较高,为50 ng/mL;特异性较好,该试纸条与黄曲霉毒素B_1、玉米赤霉烯酮、赭曲霉毒素A、T-2毒素、HT-2毒素和桔霉素未见有交叉反应;稳定性较好,25℃至少可保存5-6个月。
4对样品前处理进行了研究。结果发现,在本实验中样品颗粒大小、不同水质、搅拌时间和不同静置时间等对试纸条的检测结果无明显影响。考虑到现场快速检测情况,称取粉碎1-2 min后的样品5 g,加入100 mL纯净水或自来水提取,用玻璃棒剧烈搅拌2 min,静置2 min,进行检测,10 min后判读结果,整个过程只需15 min。
5采用自制的DON快速检测试纸条和Ridascreen Fast ELISA试剂盒分别检测了市售的小麦和玉米样品,对检测结果进行比较和分析,实验显示,两种方法的检测结果一致。
Red yeast rice is produced by growing Monascus sp.on rice to produce a red-colored product.Although for years it has been known that there are six pigments and other metabolic products from Monascus sp.,such as alcohols,organic acids,and substances with a wide range of biological and therapeutic benefits,including anticarcinogenic,antioxidative,and hypolipidemic activities,which have been described,in the past decade,some new pigments and metabolites have been isolated and their chemical structures have been characterized. However,some fluorescent compound products from Monascus sp.have received less attention.Therefore,the first part in this study,two new Monascus metabolites from red yeast rice were studied.
1 Two new Monascus metabolites with similar fluorescence spectra(λex=396 nm,λem=460 nm) and UV absorption spectra were detected.They were isolated by rechromatography on a silica gel column and semipreparative HPLC,and two strong blue fluorescent compounds were obtained.Their structures were elucidated by electrospray ionization mass spectrometry(ESI-MS),electrospray ionization tandem mass spectrometry(ESI-MS/MS), intensive ESI-MS,and nuclear magnetic resonance spectroscopy(1H NMR,13C NMR,COSY, and HMBC) studies.High-resolution mass spectrometry indicated the molecular formulas C_(21)H_(24)O_5 and C_(23)H_(28)O_5.The two new compounds,named monasfluore A(MFA) and monasfluore B(MFB),respectively,contain a alkyl side chain,γ-lactone,and propenyl group, whereas themore lipophilic compound,MFB,is a higher homologue of MFA,with the more lipophilic octanoyl instead of the hexanoyl side chain.
2 A specific HPLC method has been developed and validated for the simultaneous determination of MFA and MFB in red yeast rice.Chromatographic separation was achieved at room temperature using a 250×4.6 mm I.D.,5μm Symmetry C_(18) column(Waters),with isocratic elution of water/acetonitrile(23:77,v/v) at a flow rate of 0.8 mL/min.The average recoveries of the method for MFA and MFB were 85.2%and 82.3%,respectively,and the RSD were 4.2%and 5.3%,respectively.The linear equations of MFA and MFB were Y=772.5X-289.2 and Y=2376.6X+1346.4 respectively,and the correlation coefficients were 0.9994 and 0.9972,respectively.The linear ranges of MFA and MFB were from 0.5 to 10 ng/mL and from 0.25 to 5 ng/mL,respectively.20 samples of red yeast rice were analyzed directly by this method.The results showed that the maximum production of MFA and MFB by NO.13 Monascus sp.were 81.4 and 26.3 g/kg,respectively,and the minimum production of MFA and MFB by NO.14 Monascus sp.were 0.01 and 0.003 g/kg,respectively.
3 The stabilties of MFA and MFB for strong acid,strong alkali,heat and light were studied, and the interaction between BSA and MFA and MFB were also studied.The results showed that the stabilties of MFA and MFB for alkali,heat,light were poor,but the stabilties of MFA and MFB for strong acid were better than for strong alkali.MFA is a lower homologue of MFB,with the less lipophilic hexanoyl instead of octanoyl side chain,and this results in a less interaction with BSA.
4 The inhibition proliferation of cancer cell lines,Hep G2 and A549,and human normal cell lines,WI-38,were determined by methyl thiazolyl tetrazolium(MTT) assay method.The results indicate that the notable inhibition proliferation on A549 and Hep G2 are found in MFA and MFB,but without too significant inhibition toward normal fibroblasts WI-38 at the same concentrations of 5-20μg/mL.The concentrations of 50%percent inhibition(IC_(50)) of MFA in the two tumor cell lines(HepG2 and A549),were found to be around 12.4 and 16.3μg/mL, respectively,and IC_(50) of MFB in HepG2 and A549 were about 7.1 and 10.6μg/mL These results indicate that the length of the saturated side chain on the ketonic carbonyl group of MFB is an important factor toward the inhibition proliferation.
Deoxynivalenol(DON) is produced largely by Fusarium fungi,which are widespread in nature and commonly contaminate many cereal grains such as wheat,corn,barley,oats,and rye intended for human and animal consumption.At present,the determination of DON is normally carried out using gas chromatography(GC) with either electron capture or mass spectrometric(MS) detection,or high-performance liquid chromatography(HPLC) with ultraviolet(UV) detection,fluorescence detection after postcolumn derivatization or MS detection.The merit of chromatographic methods is that they allow highly sensitive measurements of individual toxins simultaneously.But they are thought to be unsuitable for measuring many samples within a short time,because lengthy sample preparation such as column cleanup and derivation is required to achieve high sensitivity.Furthermore, high-priced measurement machines and highly qualified personnel are required in order to apply these methods,and the running costs are generally high.In addition,some researchers have established enzyme-linked immunosorbent assay(ELISA) for DON,and it is also unsuitable for on-site detection because it requires labor-intensive operations including incubation,washing,and enzymatic reactions during signal generation.
There is a need for rapid and cheap but reliable methods that can be conducted and interpreted by users who are close to the site of contamination.Therefore,the second part in this study,a colloidal gold immunochromatographic strip(ICS) test for rapid detection of DON in wheat and maize samples was developed.
1 For the development of a sensitive ICS test,it is necessary for the optimal pH and amount of antibody for the labeled gold colloid.After centrifugation,the titer of supernatant and original antibody was compared by ELISA to determine the optimal pH value.The minimum amount of anti-DON Mab was determined by adding NaCl to colloidal gold particles containing different amounts of Mab.After reaction with NaCl,a colloidal gold solution containing minimum Mab could be kept reddish or red-orange color.It was found that the optimal pH value for the labeled colloidal gold was 7.0 and the minimum amount of Mab was 30μg for 1 mL colloidal gold.
2 A total of 0.74μL per 1 cm of DON-cationic bovine serum albumin(CBSA)(0.8 mg/mL) conjugate and goat anti-mouse IgG antibody(1.0 mg/mL) were sprayed onto NC membrane(P 40) as the T and C line,and a total of 5μL/cm of colloidal gold-labelled anti-DON Mab diluted three times,was jetted on the treated conjugate pad.In addition,the nonspecific reaction was removed by adding 0.005%anion surfactant to the solution,and it appears that anion surfactant may neutralize the positive charge of the CBSA.
3 The cross-reacted rates between the DON rapid test strip and aflatoxin B1 nivalenol,T-2, HT-2,ZEN,and citrinin were poorly.The ICS test had a visual detection limit of 50 ng/mL for DON.The validity of DON rapid test strip was at least 5-6 months at 25℃.
4 The sample preparation methods for the ICS were investigated.It was found that the test results of ICS were not significantly affected by size of the sample,different water,mixing time and standing time in this experminement.To perform the test,5 g of sample was extracted in a ratio of 1:20 with water by shaking for 2 min,standing 2 min,and then the extract directly test without further cleanup steps.After 10 min,the test results were obtained, and the whole process was about 15 min.
5 Analysis of DON in wheat and maize samples revealed that data obtained from ICS test were in a good agreement with those obtained from ELISA.The results demonstrate that the ICS test can be used as a reliable,rapid,cost-effective and convenient qualitative tool for on-site screening technique of DON in wheat and maize samples.
引文
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