Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation ...Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation and direct steam distillation method. Among their composition, the main components are terpene compounds, which account for 93.926% (mass fraction, the same below) and 85.843% of essential oils extracted from Shatian shaddock peel and Sweet shaddock peel, respectively. Although nootkatone is the major contributor of shaddock characteristic scent, and its contents are 1.069% and 1.749% of essential oils from Sweet shaddock peel and Shatian shaddock peel, respectively. The results show that squeeze-steam distillation gives higher yield and good quality of essential oil and the compositions of essential oils from two kinds of shaddock peels are different, but the main contributors of the shaddock scent are the same.展开更多
基于超高效液相色谱-串联四极杆飞行时间高分辨质谱(ultra-high performance liquid chromatographytriple quadrupole-time of flight tandem mass spectrometry,UPLC-Triple-TOF MS/MS)法对巴氏杀菌乳中的磷脂成分进行分析鉴定。采用...基于超高效液相色谱-串联四极杆飞行时间高分辨质谱(ultra-high performance liquid chromatographytriple quadrupole-time of flight tandem mass spectrometry,UPLC-Triple-TOF MS/MS)法对巴氏杀菌乳中的磷脂成分进行分析鉴定。采用色谱柱ACQUITY UPLC^®BEH C18(2.1 mm×100 mm,1.7μm),以流动相A水-甲醇-乙腈(1∶1∶1,V/V)和流动相B异丙醇-乙腈(1∶1,V/V)进行梯度洗脱,在电喷雾电离正模式下采集数据。依据高分辨质谱提供的保留时间、准分子离子、二级碎片等脂质分析数据,并结合标准品碎裂方式等信息,共鉴定出磷脂分子68种。其中,磷脂酰胆碱22种,占比7.98%;磷脂酰乙醇胺17种,占比56.60%;磷脂酰丝氨酸10种,占比1.70%;磷脂酰肌醇7种,占比1.33%;鞘磷脂12种,占比32.39%。本研究采用灵敏度高、精密度及稳定性良好的UPLC-Triple-TOF MS/MS方法实现了对牛乳中磷脂的全面定性与定量分析。此方法检测出的牛乳磷脂信息完整、磷脂种类多于其他检测技术,可为牛乳的磷脂研究提供数据基础。展开更多
Liquid chromatography coupled with the triple quadrupole mass spectrometry(LC-QQQ MS)technique is the most commonly used technique for quantitative analysis.It is widely used in pharmacology,targeted metabolomics,Chin...Liquid chromatography coupled with the triple quadrupole mass spectrometry(LC-QQQ MS)technique is the most commonly used technique for quantitative analysis.It is widely used in pharmacology,targeted metabolomics,Chinese medicine quality control,and other research fields.The technique monitors only characteristic precursors and product ions through multiple reaction monitoring(MRM)mode and can detect targeted molecules in complex matrix with high specificity and sensitivity.In the present study,a diarylamide derivative diuretic was used as an example to introduce the method establishment and parameter optimization of this liquid chromatography-mass spectrometry technique.Diuretic and its internal standard could be completely separated within a 5-min gradient,and the quantitative linear range was 1–1000 ng/mL with R2=0.9996 in practical samples.This study showed that the key to the method development for LC-QQQ MS was the selection of the LC mobile phase,the elution gradient,the declustering potential,and the collision energy of compounds in MS.展开更多
[目的]建立同时检测配合饲料中64种药物的超高效液相色谱-三重四极杆串联质谱(ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry,UHPLC-MS/MS)法,提高非法添加物的检测效率。[方法]采用Waters...[目的]建立同时检测配合饲料中64种药物的超高效液相色谱-三重四极杆串联质谱(ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry,UHPLC-MS/MS)法,提高非法添加物的检测效率。[方法]采用Waters HSS T3型色谱柱(2.1 mm×100 mm,1.8μm)进行分离,流动相A为0.1%甲酸水溶液,流动相B为含0.1%甲酸的乙腈溶液,梯度洗脱,流速为0.40 mL/min,进样量为2μL;采用电喷雾离子源正离子扫描模式进行检测,多反应监测模式进行信号采集。比较4种样品提取溶剂以及2种固相萃取柱处理对目标药物的回收率,确定样品前处理的最佳方法。利用建立的UHPLC-MS/MS法对宁夏回族自治区不同来源的100批次配合饲料样品进行64种药物检测。[结果]配合饲料样品均质后,用含0.2%甲酸的乙腈水溶液(乙腈∶水=8∶2,V/V)提取,利用Oasis PRiME HLB型固相萃取柱对样品净化,多数目标药物的回收率在60%以上。64种药物在浓度为5.0~200.0μg/L的范围内线性关系良好,相关系数(R)均大于0.99;不同药物的定量限在5.0~10.0μg/kg;阳性添加5.0、20.0、50.0μg/kg 3个浓度的平均回收率在41.00%~120.49%,批内相对标准偏差(RSD)在0.54%~15.94%,批间RSD在1.25%~13.64%。在100个批次的配合饲料样品中均未检出目标药物。[结论]建立的UHPLC-MS/MS法线性关系良好、回收率高、精密度好,具有较高的重现性和较好的可操作性,可用于配合饲料中非法添加64种药物的筛查。展开更多
建立了一种μ-QuEChERS结合气相色谱-三重四极杆串联质谱仪(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)在10 min内测定桃胶中106种农药残留的方法。样品经μ-QuEChERS方法提取、净化,经超高惰性气相色谱...建立了一种μ-QuEChERS结合气相色谱-三重四极杆串联质谱仪(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)在10 min内测定桃胶中106种农药残留的方法。样品经μ-QuEChERS方法提取、净化,经超高惰性气相色谱柱(highly inert gas chromatographic column,HIGC)分离,以三重四极杆-串联质谱仪检测分析,基质标准曲线外标法定量。106种农药在0.00200~0.400 mg/kg范围,其线性相关系数R均大于0.995,对于0.500 g样品的106种农药的检出限为(5.84×10^(-6))~(2.81×10^(-3))mg/kg,定量限为(1.95×10^(-5))~(9.36×10^(-3))mg/kg,且低、中、高3个浓度添加水平的回收率为72%~109%,相对标准偏差(relative standard deviations,RSDs)为0.73%~10%。该方法具有快捷、污染小、可靠性强的特点,适用于桃胶中多种农药残留的快速定性和定量检测。展开更多
文摘Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation and direct steam distillation method. Among their composition, the main components are terpene compounds, which account for 93.926% (mass fraction, the same below) and 85.843% of essential oils extracted from Shatian shaddock peel and Sweet shaddock peel, respectively. Although nootkatone is the major contributor of shaddock characteristic scent, and its contents are 1.069% and 1.749% of essential oils from Sweet shaddock peel and Shatian shaddock peel, respectively. The results show that squeeze-steam distillation gives higher yield and good quality of essential oil and the compositions of essential oils from two kinds of shaddock peels are different, but the main contributors of the shaddock scent are the same.
基金National Natural Science Foundation of China(Grant No.22004004 and 81620108029).
文摘Liquid chromatography coupled with the triple quadrupole mass spectrometry(LC-QQQ MS)technique is the most commonly used technique for quantitative analysis.It is widely used in pharmacology,targeted metabolomics,Chinese medicine quality control,and other research fields.The technique monitors only characteristic precursors and product ions through multiple reaction monitoring(MRM)mode and can detect targeted molecules in complex matrix with high specificity and sensitivity.In the present study,a diarylamide derivative diuretic was used as an example to introduce the method establishment and parameter optimization of this liquid chromatography-mass spectrometry technique.Diuretic and its internal standard could be completely separated within a 5-min gradient,and the quantitative linear range was 1–1000 ng/mL with R2=0.9996 in practical samples.This study showed that the key to the method development for LC-QQQ MS was the selection of the LC mobile phase,the elution gradient,the declustering potential,and the collision energy of compounds in MS.
文摘建立了一种μ-QuEChERS结合气相色谱-三重四极杆串联质谱仪(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)在10 min内测定桃胶中106种农药残留的方法。样品经μ-QuEChERS方法提取、净化,经超高惰性气相色谱柱(highly inert gas chromatographic column,HIGC)分离,以三重四极杆-串联质谱仪检测分析,基质标准曲线外标法定量。106种农药在0.00200~0.400 mg/kg范围,其线性相关系数R均大于0.995,对于0.500 g样品的106种农药的检出限为(5.84×10^(-6))~(2.81×10^(-3))mg/kg,定量限为(1.95×10^(-5))~(9.36×10^(-3))mg/kg,且低、中、高3个浓度添加水平的回收率为72%~109%,相对标准偏差(relative standard deviations,RSDs)为0.73%~10%。该方法具有快捷、污染小、可靠性强的特点,适用于桃胶中多种农药残留的快速定性和定量检测。
