麦角甾醇含量检测分析柑橘真菌污染程度的方法研究
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摘要
建立了以7-去氢胆固醇为内标,气质联用(GC-MS)法同步选择离子检测/全扫描的定量检测方法,并采用该方法检测了不同程度霉变的柑橘中的麦角甾醇含量,确定柑橘的真菌污染程度。结果表明,麦角甾醇在5~200μg/m L质量浓度范围内具有良好的线性关系(R~2=0.999 9);检出限和定量限分别为3.12 mg/kg、10.39 mg/kg,加标回收率范围在91.33%~100.14%,日内相对标准偏差为0.04~0.49%、日间相对标准偏差为0.22%。该方法简便、灵敏、准确,麦角甾醇含量可作为柑橘早期受真菌侵染的重要指标。
A quantitative determination method by GC-MS with synchronize seletion ion monitoring/full scan mode was established by using 7-dehydrocholesterlo as internal standard. The contents of ergosterol in fungal-contaminated citrus with different levels were determined. The results showed that the calibration curve exhibited good linearity with a correlation coefficient R~2 of 0.999 9 in the range of 5-200 μg/ml. The limit of detection(LOD) and limit of quantitation(LOQ) were 3.12 mg/kg and 10.39 mg/kg, respectively. The adding standard recovery rate ranged from 91.33% to 100.14% with the intra-day relative standard deviation of 0.04~0.49% and inter-day relative standard deviation 0.22%. The method was simple, sensitive and accurate, and ergosterol contents could be as an important indicator in early fungal-contaminated citrus.
A quantitative determination method by GC-MS with synchronize seletion ion monitoring/full scan mode was established by using 7-dehydrocholesterlo as internal standard. The contents of ergosterol in fungal-contaminated citrus with different levels were determined. The results showed that the calibration curve exhibited good linearity with a correlation coefficient R~2 of 0.999 9 in the range of 5-200 μg/ml. The limit of detection(LOD) and limit of quantitation(LOQ) were 3.12 mg/kg and 10.39 mg/kg, respectively. The adding standard recovery rate ranged from 91.33% to 100.14% with the intra-day relative standard deviation of 0.04~0.49% and inter-day relative standard deviation 0.22%. The method was simple, sensitive and accurate, and ergosterol contents could be as an important indicator in early fungal-contaminated citrus.
引文
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[13]何学超,郭道林,兰盛斌,等.粮食中麦角甾醇含量正相液相色谱法检测[J].粮食储藏,2008,37(2):43-46.
[14]刘晶京,黄文华,吕明亮,等.HPLC法测定不同品种及段木栽培灵芝子实体中麦角甾醇含量[J].中药材,2011,34(2):187-190.
[15]邓婧,黄宏南,林宏琳.高效液相色谱-二极管阵列检测法测定游离麦角甾醇的含量[J].海峡预防医学杂志,2011,17(1):56-58.
[16]刘云花,李辉章,姜涛,等.影响液相色谱检测麦角甾醇结果的因素[J].粮油仓储科技通讯,2012,36(2):41-42.
[17]单慰曾,陆斌,徐霞,等.紫外光谱检测香菇液体和固体菌丝麦角甾醇[J].植物生理学通讯,1989(2):67-70.
[18]LEEFMANN T,HEIM C,SILJESTR魻M S,et al.Spectral characterization of ten cyclic lipids using time-of-flight secondary ion mass spectrometry[J].Rapid Commun Mass Sp,2013,27(5):565-581.
[19]何学超,郭道林,兰盛斌,等.麦角甾醇可作为评价粮食质量安全的敏感指标之一[J].粮食储藏,2007,36(6):22-26.
[2]张恒,许兆棠,李文谦,等.还原糖及维生素C含量变化与香蕉霉变进程的关系[J].中国南方果树,2012,41(2):71-74.
[3]周亮,杨文侠,钟八莲,等.赣南脐橙贮藏期间霉变病菌分离及抑菌实验研究[J].赣南师范学院学报,2013,34(3):45-49.
[4]张大为,张洁,李猛.分离引起柑橘腐烂、霉变的微生物及生物防治[J].生物加工过程,2011,9(4):54-57.
[5]王春红.柿饼霉变及其防霉技术研究[D].西安:陕西师范大学,2010.
[6]李冬娟.酿造用原辅料中霉菌的分离鉴定及霉变原辅料对发酵产品品质和安全性的影响[D].西安:西北大学,2010.
[7]张楠楠.基于嵌入式系统的粮食霉变检测装置研究[D].淄博:山东理工大学,2014.
[8]朱建云,赵德安,潘天红,等.基于人工嗅觉的粮食霉变识别方法的研究[J].农业工程学报,2005,21(1):106-109.
[9]JOHANNES R,ERLAND B.Growth of saprotrophic fungi and bacteria in soil[J].FEMS Microbiol Ecol,2011,78(1):17-30.
[10]TANG W,KUEHN T H,SIMCIK M F.Effects of temperature,humidity and air flow on fungal growth rate on loaded ventilation filters[J].J Occup Environ Hyg,2015,12(8):525-537.
[11]TAIPALE S J,HILTUNEN M,VUORIO K,et al.Suitability of phytosterols alongside fatty acids as chemotaxonomic biomarkers for phytoplankton[J].Front Plant Sci,2016,7:1-16.
[12]曹龙辉,李晓珺,赵文红,等.麦角甾醇的研究进展[J].中国酿造,2014,33(4):9-12.
[13]何学超,郭道林,兰盛斌,等.粮食中麦角甾醇含量正相液相色谱法检测[J].粮食储藏,2008,37(2):43-46.
[14]刘晶京,黄文华,吕明亮,等.HPLC法测定不同品种及段木栽培灵芝子实体中麦角甾醇含量[J].中药材,2011,34(2):187-190.
[15]邓婧,黄宏南,林宏琳.高效液相色谱-二极管阵列检测法测定游离麦角甾醇的含量[J].海峡预防医学杂志,2011,17(1):56-58.
[16]刘云花,李辉章,姜涛,等.影响液相色谱检测麦角甾醇结果的因素[J].粮油仓储科技通讯,2012,36(2):41-42.
[17]单慰曾,陆斌,徐霞,等.紫外光谱检测香菇液体和固体菌丝麦角甾醇[J].植物生理学通讯,1989(2):67-70.
[18]LEEFMANN T,HEIM C,SILJESTR魻M S,et al.Spectral characterization of ten cyclic lipids using time-of-flight secondary ion mass spectrometry[J].Rapid Commun Mass Sp,2013,27(5):565-581.
[19]何学超,郭道林,兰盛斌,等.麦角甾醇可作为评价粮食质量安全的敏感指标之一[J].粮食储藏,2007,36(6):22-26.