Analysis of Flavonoids in Dalbergia odorifera by Ultra-Performance Liquid Chromatography with Tandem Mass Spectrometry

Dalbergia odorifera, a traditional Chinese medicine, has been used to treat cardio- and cerebrovascular diseases in China for thousands of years. Flavonoids are major active compounds in D. odorifera. In this paper, a rapid and sensitive ultra-high performance liquid chromatography-triple quadrupole mass spectrometry method was developed and validated for simultaneous determination of 17 flavonoids in D. odorifera. Quantification was performed by multiple reaction monitoring using electrospray ionization in negative ion mode. Under the optimum conditions, calibration curves for the 17 analytes displayed good linearity (r2 > 0.9980). The intra- and inter-day precisions (relative standard deviations) were lower than 5.0%. The limit of quantitation ranged from 0.256 to 18.840 ng/mL. The mean recovery range at three spiked concentrations was 94.18–101.97%. The validated approach was successfully applied to 18 samples of D. odorifera. Large variation was observed for the contents of the 17 analytes. Sativanone and 3′-O-methylviolanone were the dominant compounds. The fragmentation behaviors of six flavonoids were investigated using UPLC with quadrupole time-of-flight tandem mass spectrometry. In negative ion electrospray ionization mass spectrometry, all the flavonoids yielded prominent [M − H]− ions. Fragments for losses of CH3, CO, and CO2 were observed in the mass spectra. Formononetin, liquiritigenin, isoliquiritigenin, sativanone, and alpinetin underwent retro-Diels–Alder fragmentations. The proposed method will be helpful for quality control of D. odorifera.

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Detection and Identification of Zeranol in Chicken or Rabbit Liver by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

Journal of AOAC International ◽

10.1093/jaoac/85.4.841 ◽

2002 ◽

Vol 85 (4) ◽

pp. 841-847 ◽

Cited By ~ 11

Author(s):

Xiaoming Fang ◽

Jiahua Chen ◽

Dehua Guo ◽

Guoquan Wang

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Multiple Reaction Monitoring ◽

Rabbit Liver ◽

Negative Ion ◽

Tandem Mass ◽

Detection And Identification ◽

Relative Standard ◽

Limit Of Quantitation

Abstract A sensitive, specific, and reliable liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for detection and identification of zeranol in chicken or rabbit liver. A homogenized liver sample was hydrolyzed with β-glucuronidase/arylsulfatase, and the hydrolysate was extracted with ethyl ether. The supernatant was evaporated to dryness, and the residue was dissolved in chloroform and re-extracted with sodium hydroxide. After acidification, the extract was cleaned up on a C18 solid-phase extraction cartridge and analyzed by electrospray LC-MS/MS in the negative ion mode. The multiple reaction monitoring transition from both m/z 321 to 277 and m/z 321 to 303 was monitored for confirmation, and the product ion of 277 was used for quantitation. Separation was performed on a Waters XTettra™ C18 column (50 × 2.1 mm, 3.5 μm) combined with a safeguard column (Symmetry C18, 20 × 3.9 mm, 5 μm), using a gradient elution with acetonitrile and 20mM ammonium acetate. Calibration curves were prepared and good linearity was achieved over the concentration ranges tested. For all liver samples fortified at 3 different levels of 1, 5, and 50 μg/kg, the overall recoveries and relative standard deviations were in the range of 61–90 and 8–13%, respectively. The limit of quantitation based on the assay validation was 1 μg/kg. The method had been used on a routine basis for detection and identification of zeranol in liver samples.

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Determination of Deltamethrin Residues in Plant Materials by Liquid Chromatography/Tandem Mass Spectrometry with Electrospray Ionization

Journal of AOAC International ◽

10.1093/jaoac/89.3.786 ◽

2006 ◽

Vol 89 (3) ◽

pp. 786-796 ◽

Cited By ~ 5

Author(s):

Dieter Zimmer ◽

Christiane Philipowski ◽

Birgit Posner ◽

Agnes Gnielka ◽

Edgar Dirr ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Electrospray Ionization ◽

Tandem Mass ◽

Chromatography Tandem Mass Spectrometry ◽

Relative Standard ◽

Limit Of Quantitation ◽

Liquid Chromatography Tandem Mass

Abstract This paper describes a selective and sensitive method that uses liquid chromatography/tandem mass spectrometry with positive electrospray ionization (ESI+) for the determination of deltamethrin in a variety of crops. Samples were extracted by conventional high-speed blending. Some samples required no further cleanup; others were cleaned up by gel permeation chromatography, strong cation-exchange cartridges, or partitioning with n-hexane. In the determinative step, the buffered neutral mobile phase, consisting of 10 mM ammonium acetate (pH 6.8) and methanol, and ESI+ provided strong ammonium adduct formation to [M+NH4]+ at m/z 523, and the multiple-reaction monitoring (MRM) transition at m/z 523/281 was used for the quantitation of deltamethrin. A second MRM transition at m/z 525/283 was used for confirmation. The limit of quantitation (LOQ) values were 0.01 mg/kg for edible materials and 0.05 mg/kg for nonedible materials. Mean overall recoveries at the LOQ and the 10-fold LOQ ranged from 73 to 96%, and the relative standard deviations were <10% for all samples materials analyzed.

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Dried Urine Microsampling Coupled to Liquid Chromatography—Tandem Mass Spectrometry (LC–MS/MS) for the Analysis of Unconjugated Anabolic Androgenic Steroids

Molecules ◽

10.3390/molecules25143210 ◽

2020 ◽

Vol 25 (14) ◽

pp. 3210 ◽

Cited By ~ 1

Author(s):

Michele Protti ◽

Camilla Marasca ◽

Marco Cirrincione ◽

Angelo E. Sberna ◽

Roberto Mandrioli ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Anabolic Androgenic Steroids ◽

Tandem Mass ◽

Chromatography Tandem Mass Spectrometry ◽

Relative Standard ◽

Limit Of Quantitation ◽

Liquid Chromatography Tandem Mass ◽

Androgenic Steroids

Testing and monitoring anabolic androgenic steroids in biological fluids is a key activity in anti-doping practices. In this study, a novel approach is proposed, based on dried urine microsampling through two different workflows: dried urine spots (DUS) and volumetric absorptive microsampling (VAMS). Both techniques can overcome some common drawbacks of urine sampling, such as analyte instability and storage and transportation problems. Using an original, validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) method, exogenous and endogenous unconjugated steroids were analysed. Despite the limitations of microsampling volume, good sensitivity was obtained (limit of quantitation ≤1.5 ng/mL for all analytes), with satisfactory precision (relative standard deviation <7.6%) and absolute recovery (>70.3%). Both microsampling platforms provide reliable results, in good agreement with those obtained from urine.

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