This work first describes a simple approach for the untargeted profiling of volatile compounds for distinguishing between white duck down (WDD) and white goose down (WGD) based on resolution-optimized GC-IMS combined ...This work first describes a simple approach for the untargeted profiling of volatile compounds for distinguishing between white duck down (WDD) and white goose down (WGD) based on resolution-optimized GC-IMS combined with optimized chemometric techniques, namely PCA. The detection method for down samples was established by using GC-IMS. Meanwhile, the reason of unpleasant odors caused by WDD was explained on the basis of the characteristic volatile compounds identification. GC-IMS fingerprinting can be considered a revolutionary approach for a truly fully automatable, cost-efficient, and in particular highly sensitive method. A total of 22 compounds were successfully separated and identified through GC-IMS method, and the significant differences in volatile compounds were observed in three parts of WDD and WGD samples. The most characteristic volatile compounds of WGD belong to aldehydes, whereas carboxylic acids from WDD were detected generated by autoxidation reaction. Meanwhile, the main reason of unpleasant odor generation was possibly attributed to the high concentration of volatile carboxylic acids of WDD. Therefore, the constructed model presents a simple and efficient method of analysis and serves as a basis for down processing and quality control.展开更多
The complex composition of herbal metabolites necessitates the development of powerful analytical techniques aimed to identify the bioactive components.The seeds of Descurainia sophia(SDS)are utilized in China as a co...The complex composition of herbal metabolites necessitates the development of powerful analytical techniques aimed to identify the bioactive components.The seeds of Descurainia sophia(SDS)are utilized in China as a cough and asthma relieving agent.Herein,a dimension-enhanced integral approach,by combining ultra-high performance liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(UHPLC/IMQTOF-MS)and intelligent peak annotation,was developed to rapidly characterize the multicomponents from SDS.Good chromatographic separation was achieved within 38 min on a UPLC CSH C18(2.1×100 mm,1.7μm)column which was eluted by 0.1%formic acid in water(water phase)and acetonitrile(organic phase).Collision-induced dissociation-MS^(2)data were acquired by the data-independent high-definition MS^(E)(HDMS^(E))in both the negative and positive electrospray ionization modes.A major components knockout strategy was applied to improve the characterization of those minor ingredients by enhancing the injection volume.Moreover,a self-built chemistry library was established,which could be matched by the UNIFI software enabling automatic peak annotation of the obtained HDMS^(E)data.As a result of applying the intelligent peak annotation workflows and further confirmation process,a total of 53 compounds were identified or tentatively characterized from the SDS,including 29 flavonoids,one uridine derivative,four glucosides,one lignin,one phenolic compound,and 17 others.Notably,four-dimensional information related to the structure(e.g.,retention time,collision cross section,MS^(1)and MS^(2)data)was obtained for each component by the developed integral approach,and the results would greatly benefit the quality control of SDS.展开更多
The standards of plant toxins were separated by a C18 column with gradient elution with 0.1% formic acid/water (V/V) and 0.1% formic acid/acetonitrile (V/V) as mobile phase and acquired by ion mobility-quadrupole time...The standards of plant toxins were separated by a C18 column with gradient elution with 0.1% formic acid/water (V/V) and 0.1% formic acid/acetonitrile (V/V) as mobile phase and acquired by ion mobility-quadrupole time of flight mass spectrometry (IM-QTOF MS) in positive ion mode. A database of 308 plant toxins including retention time, collision cross-section (CCS) and its fragment ions was established. Honey dissolved in water or herbal beverage was extracted by acetonitrile and purified with PSA sorbent, and then acquired by ultrahigh-performance liquid chromatography IM-QTOFMS. The acquired data were processed by comparing with the database we established to confirm the target compounds. The average recoveries for samples at two levels ranged from 60.6% - 120.1%, with relative standard deviation (n = 6) less than 25%. The limit of quantitation for plant toxins ranged from 1 - 20 μg/kg. The developed screening method was used in determination of honey, herbal beverage and honey flavored tea beverage samples. The results showed that berberine was detected in one honey with 1 μg/kg and caffeine was present in some beverages with the concentration from 200 and 5500 μg/kg. This method could meet the requirement for rapid screening of plant toxins in honey and herbal beverage. It can be used for the quality control of honey and herbal beverage in enterprises or quality inspection departments. It also can be used in the rapid screening of food poisoning.展开更多
目的探究不同肉酱比对鹿肉酱中挥发性有机化合物(volatile organic compounds,VOCs)影响的差异性,并筛选不同肉酱比的关键性VOCs。方法利用电子鼻结合气相色谱-离子迁移谱法(gas chromatography-ion mobility spectrometry,GC-IMS)检测...目的探究不同肉酱比对鹿肉酱中挥发性有机化合物(volatile organic compounds,VOCs)影响的差异性,并筛选不同肉酱比的关键性VOCs。方法利用电子鼻结合气相色谱-离子迁移谱法(gas chromatography-ion mobility spectrometry,GC-IMS)检测不同肉酱比加工的鹿肉酱样品中的香气类别及VOCs成分,通过计算偏最小二乘法判别(partial least squares discriminant analysis,PLS-DA)和正交-偏最小二乘法判别(orthogonal partial least squares discriminant analysis,OPLS-DA)分析变量重要性因子(variable important for the projection,VIP),筛选可区分不同肉酱比的鹿肉酱样品中差异性影响最关键的变量敏感物质及VOCs(VIP>1)。结果电子鼻传感器S3、S7、S9和S10对应的氨类、芳香族、硫化物和萜烯类、芳香族、硫化氢类、烷烃类等敏感物质是不同肉酱比的鹿肉酱样品中最关键的挥发类特征性气味;利用GC-IMS共检测出82种主要VOCs,筛选出33种关键差异性特征VOCs(VIP>1),与电子鼻的关键特征性香气检测结果一致。结论基于电子鼻和GC-IMS的主要特征香气标志物的聚类分析能够有效、全面、客观地对不同肉酱比的鹿肉酱中关键挥发性性气味和VOCs进行区分和评价。展开更多
目的优化黑参甜米酒加工工艺,测定其挥发性成分。方法以黑参添加量、甜酒曲添加量、发酵时间、发酵温度进行单因素试验,通过正交试验确定最佳工艺。结果在黑参添加量为4%、甜酒曲添加量为2.0%、发酵温度30℃、发酵时间为72 h时的条件下...目的优化黑参甜米酒加工工艺,测定其挥发性成分。方法以黑参添加量、甜酒曲添加量、发酵时间、发酵温度进行单因素试验,通过正交试验确定最佳工艺。结果在黑参添加量为4%、甜酒曲添加量为2.0%、发酵温度30℃、发酵时间为72 h时的条件下感官评分最高,酒精度为15%vol,其理化指标及微生物指标符合相关标准。所得黑参甜米酒酒香浓郁并伴有黑参特有的香气,口感醇厚、色泽清亮。通过顶空-气相色谱-离子迁移谱法(headspace gas chromatography ion mobility spectrometry,HS-GC-IMS)分析,共鉴定出36个挥发性成分,其中成分明确的有29种,酸类6种、烃类2种、醇类6种、酯类4种、酚类1种、醛类7种、酮类3种。结论以黑参和糯米为原料制备黑参甜米酒,通过对黑参米酒加工工艺的优化,得到适宜的加工条件,通过HS-GC-IMS测定米酒中的挥发性成分,为新型米酒成分的分析提供参考,为米酒赋予黑参特有的保健功能。展开更多
文摘This work first describes a simple approach for the untargeted profiling of volatile compounds for distinguishing between white duck down (WDD) and white goose down (WGD) based on resolution-optimized GC-IMS combined with optimized chemometric techniques, namely PCA. The detection method for down samples was established by using GC-IMS. Meanwhile, the reason of unpleasant odors caused by WDD was explained on the basis of the characteristic volatile compounds identification. GC-IMS fingerprinting can be considered a revolutionary approach for a truly fully automatable, cost-efficient, and in particular highly sensitive method. A total of 22 compounds were successfully separated and identified through GC-IMS method, and the significant differences in volatile compounds were observed in three parts of WDD and WGD samples. The most characteristic volatile compounds of WGD belong to aldehydes, whereas carboxylic acids from WDD were detected generated by autoxidation reaction. Meanwhile, the main reason of unpleasant odor generation was possibly attributed to the high concentration of volatile carboxylic acids of WDD. Therefore, the constructed model presents a simple and efficient method of analysis and serves as a basis for down processing and quality control.
基金This work was financially supported by the National Key Research and Development Program of China(Grant No.2018YFC1704500)Tianjin Committee of Science and Technology of China(Grant No.21ZYJDJC00080)National Natural Science Foundation of China(Grant No.81872996).
文摘The complex composition of herbal metabolites necessitates the development of powerful analytical techniques aimed to identify the bioactive components.The seeds of Descurainia sophia(SDS)are utilized in China as a cough and asthma relieving agent.Herein,a dimension-enhanced integral approach,by combining ultra-high performance liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(UHPLC/IMQTOF-MS)and intelligent peak annotation,was developed to rapidly characterize the multicomponents from SDS.Good chromatographic separation was achieved within 38 min on a UPLC CSH C18(2.1×100 mm,1.7μm)column which was eluted by 0.1%formic acid in water(water phase)and acetonitrile(organic phase).Collision-induced dissociation-MS^(2)data were acquired by the data-independent high-definition MS^(E)(HDMS^(E))in both the negative and positive electrospray ionization modes.A major components knockout strategy was applied to improve the characterization of those minor ingredients by enhancing the injection volume.Moreover,a self-built chemistry library was established,which could be matched by the UNIFI software enabling automatic peak annotation of the obtained HDMS^(E)data.As a result of applying the intelligent peak annotation workflows and further confirmation process,a total of 53 compounds were identified or tentatively characterized from the SDS,including 29 flavonoids,one uridine derivative,four glucosides,one lignin,one phenolic compound,and 17 others.Notably,four-dimensional information related to the structure(e.g.,retention time,collision cross section,MS^(1)and MS^(2)data)was obtained for each component by the developed integral approach,and the results would greatly benefit the quality control of SDS.
文摘The standards of plant toxins were separated by a C18 column with gradient elution with 0.1% formic acid/water (V/V) and 0.1% formic acid/acetonitrile (V/V) as mobile phase and acquired by ion mobility-quadrupole time of flight mass spectrometry (IM-QTOF MS) in positive ion mode. A database of 308 plant toxins including retention time, collision cross-section (CCS) and its fragment ions was established. Honey dissolved in water or herbal beverage was extracted by acetonitrile and purified with PSA sorbent, and then acquired by ultrahigh-performance liquid chromatography IM-QTOFMS. The acquired data were processed by comparing with the database we established to confirm the target compounds. The average recoveries for samples at two levels ranged from 60.6% - 120.1%, with relative standard deviation (n = 6) less than 25%. The limit of quantitation for plant toxins ranged from 1 - 20 μg/kg. The developed screening method was used in determination of honey, herbal beverage and honey flavored tea beverage samples. The results showed that berberine was detected in one honey with 1 μg/kg and caffeine was present in some beverages with the concentration from 200 and 5500 μg/kg. This method could meet the requirement for rapid screening of plant toxins in honey and herbal beverage. It can be used for the quality control of honey and herbal beverage in enterprises or quality inspection departments. It also can be used in the rapid screening of food poisoning.
文摘目的探究不同肉酱比对鹿肉酱中挥发性有机化合物(volatile organic compounds,VOCs)影响的差异性,并筛选不同肉酱比的关键性VOCs。方法利用电子鼻结合气相色谱-离子迁移谱法(gas chromatography-ion mobility spectrometry,GC-IMS)检测不同肉酱比加工的鹿肉酱样品中的香气类别及VOCs成分,通过计算偏最小二乘法判别(partial least squares discriminant analysis,PLS-DA)和正交-偏最小二乘法判别(orthogonal partial least squares discriminant analysis,OPLS-DA)分析变量重要性因子(variable important for the projection,VIP),筛选可区分不同肉酱比的鹿肉酱样品中差异性影响最关键的变量敏感物质及VOCs(VIP>1)。结果电子鼻传感器S3、S7、S9和S10对应的氨类、芳香族、硫化物和萜烯类、芳香族、硫化氢类、烷烃类等敏感物质是不同肉酱比的鹿肉酱样品中最关键的挥发类特征性气味;利用GC-IMS共检测出82种主要VOCs,筛选出33种关键差异性特征VOCs(VIP>1),与电子鼻的关键特征性香气检测结果一致。结论基于电子鼻和GC-IMS的主要特征香气标志物的聚类分析能够有效、全面、客观地对不同肉酱比的鹿肉酱中关键挥发性性气味和VOCs进行区分和评价。
文摘目的优化黑参甜米酒加工工艺,测定其挥发性成分。方法以黑参添加量、甜酒曲添加量、发酵时间、发酵温度进行单因素试验,通过正交试验确定最佳工艺。结果在黑参添加量为4%、甜酒曲添加量为2.0%、发酵温度30℃、发酵时间为72 h时的条件下感官评分最高,酒精度为15%vol,其理化指标及微生物指标符合相关标准。所得黑参甜米酒酒香浓郁并伴有黑参特有的香气,口感醇厚、色泽清亮。通过顶空-气相色谱-离子迁移谱法(headspace gas chromatography ion mobility spectrometry,HS-GC-IMS)分析,共鉴定出36个挥发性成分,其中成分明确的有29种,酸类6种、烃类2种、醇类6种、酯类4种、酚类1种、醛类7种、酮类3种。结论以黑参和糯米为原料制备黑参甜米酒,通过对黑参米酒加工工艺的优化,得到适宜的加工条件,通过HS-GC-IMS测定米酒中的挥发性成分,为新型米酒成分的分析提供参考,为米酒赋予黑参特有的保健功能。
