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建立了超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用(UPLC-LTQ/Orbitrap MS)快速筛查、定性识别化妆品中24种激素的分析方法。不同剂型的化妆品样品经甲醇超声提取,用Waters ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7 μm)分离,以乙腈和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱。通过静电场轨道阱全扫描得到激素化合物的准分子离子的精确质量数,实现对化妆品中激素的快速筛查;再以保留时间和数据依赖扫描(data dependent scan)模式获得的子离子质谱图进行定性确证。24种激素化合物的质量准确度误差小于3×10-6(3 ppm);线性良好,相关系数大于0.99;检出限≤10 μg/kg(S/N=3),能满足实际化妆品样品的分析要求。应用该方法对不同剂型的50余种化妆品样品进行筛查分析,结果良好。该方法是化妆品中激素快速筛查、定性识别的有效方法。 相似文献
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Jürgen Schmidt 《Journal of mass spectrometry : JMS》2016,51(1):33-43
Representative compounds with a 1,3‐dihydroxybenzene substructure belonging to different important polyphenol classes (stilbenes, flavones, isoflavones, flavonols, flavanones, flavanols, phloroglucinols, anthraquinones and bisanthraquinones) were investigated based on detailed high‐resolution tandem mass spectrometry measurements with an Orbitrap system under negative ion electrospray conditions. The mass spectral behaviour of these compound classes was compared among each other not only with respect to previously described losses of CO, CH2CO and C3O2 but also concerning the loss of CO2 and successive specific fragmentations. Furthermore, some unusual fragmentations such as the loss of a methyl radical during mass spectral decomposition are discussed. The obtained results demonstrate both similarities and differences in their mass spectral fragmentation under MSn conditions, allowing a characterization of the corresponding compound type. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
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Kai Schuhmann Reinaldo Almeida Mark Baumert Ronny Herzog Stefan R. Bornstein Andrej Shevchenko 《Journal of mass spectrometry : JMS》2012,47(1):96-104
Top–down shotgun lipidomics relies on direct infusion of total lipid extracts into a high‐resolution tandem mass spectrometer and implies that individual lipids are recognized by their accurately determined m/z. Lipid ionization efficiency and detection specificity strongly depend on the acquisition polarity, and therefore it is beneficial to analyze lipid mixtures in both positive and negative modes. Hybrid LTQ Orbitrap mass spectrometers are widely applied in top–down lipidomics; however, rapid polarity switching was previously unfeasible because of the severe and immediate degradation of mass accuracy. Here, we report on a method to rapidly acquire high‐resolution spectra in both polarity modes with sub‐ppm mass accuracy and demonstrate that it not only simplifies and accelerates shotgun lipidomics analyses but also improves the lipidome coverage because more lipid classes and more individual species within each class are recognized. In this way, shotgun analysis of total lipid extracts of human blood plasma enabled to quantify 222 species from 15 major lipid classes within 7 min acquisition cycle. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Simultaneous determination of usnic,diffractaic, evernic and barbatic acids in rat plasma by ultra‐high‐performance liquid chromatography–quadrupole exactive Orbitrap mass spectrometry and its application to pharmacokinetic studies
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《Biomedical chromatography : BMC》2018,32(3)
Usnea longissima Ach. (Usnea) is used in pharmaceuticals, food and cosmetics. Evernic acid (EA), barbatic acid (BA), diffractaic acid (DA) and usnic acid (UA) are the most typical ingredients in U. longissima and exert a wide variety of biological functions. The study aimed to develop a sensitive method for simultaneous analysis of EA, BA, DA and UA in rat plasma and was applied to pharmacokinetic studies after consumption of UA and ethanol extract from U. longissima (UE). The samples were separated on a BEH C18 column by gradient elution with 0.5% formic acid in water and in methanol. The relative molecular masses of analytes were obtained in full‐scan range from 50.0 to 750.0 m/z under negative ionization mode by UPLC‐Q‐Exactive Orbitrap MS. All validation parameters, such as lower limit of quantitation, linearity, specificity, precision, accuracy, extraction recovery, matrix effect and stability, were within acceptable ranges and the method was appropriate for biological specimen analysis. The pharmacokinetic results indicated that the absolute bioavailabilities of UA after oral administration of UA and UE reached 69.2 and 146.9%, respectively. Compared with UA in UE, the relative bioavailability of DA, BA and EA reached 103.7, 10.4 and 0.7% after oral administration of UE. 相似文献
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Zhanpeng Shang Lulu Xu Haidong Wang Long Sun Tao Bo Min Ye Xue Qiao 《Journal of separation science》2020,43(17):3391-3398
Acylated compounds are often present in herbal medicines. In this study, a diagnostic product ion‐based strategy was established to comprehensively characterize acylated compounds in Scrophulariae Radix. After untargeted data acquisition using ultra‐high performance liquid chromatography coupled with Orbitrap mass spectrometry, the data were processed by three‐stage diagnostic product ions. First, diagnostic product ions corresponding to the acyl groups (cinnamoyl, p‐coumaroyl, feruloyl, and caffeoyl) were used to search 90 compounds. Second, these compounds were divided into three categories using diagnostic product ions for phenylethanoid glycosides, iridoid glycosides, and phenylpropanoids, respectively. Last, the linkage position of the acyl group to iridoid glycosides was discriminated via the third‐stage diagnostic product ions. As a result, 90 acylated compounds were characterized, and 37 of them were reported from Scrophulariae Radix for the first time. 相似文献
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Rita Celano Imma Pagano Sonia Carabetta Rosa Di Sanzo Luca Rastrelli 《Natural product research》2019,33(2):244-251
Consumers are aware of diet causing health problems and therefore there is an increased demand for natural ingredients that are expected to be safe and health-promoting. Many of these compounds belong to the class of flavonoids and can be divided into these five groups: flavanones, flavones, flavonols, flavanols, isoflavones and anthocyanidins. Extracts from citrus fruits are usually used as functional ingredients for several products. The aim of this paper was to develop an UHPLC-UV-ESI-HRMS method to define the metabolite profile of different parts of citrus fruit, of a particular cultivar called ‘Ovale Calabrese’, and in its main by-products. The high resolution mass spectrometry analysis allowed the identification of 27 compounds belonging to the classes of flavonoids and terpenoids. The high contents of phytochemical compounds, reveal the potential use of the ‘Ovale Calabrese’ as a rich source of nutraceutical compounds. 相似文献
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《Biomedical chromatography : BMC》2017,31(11)
A quick, easy, effective method followed by ultra‐high‐pressure liquid chromatography coupled with linear ion trap–Orbitrap tandem mass spectrometry (UHPLC‐LTQ‐Orbitrap MS) was developed for the simultaneous identification and quantification of the metabolites produced by amentoflavone (AMF) in human intestinal bacteria from human feces. The method validated for quantification of AMF concerning precision, accuracy, recovery, matrix effect, stability and limits showed acceptable results. Compared with blank human intestinal bacteria chromatography, three metabolites were identified based on high‐accuracy protonated precursors and multi‐stage mass spectrometry (MSn ) using the proposed strategy. At the same time, a new method was developed for semi‐quantification of three metabolites. We describe the trend over 24 h of concentration–time curves for AMF and its metabolites. Moreover, the main metabolic pathway of AMF was clarified in human intestinal bacteria. The method was validated and successfully applied to the detection and quantification of AMF and its metabolites. 相似文献