, 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
. 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
. 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 (
> 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
. Large variation was observed for the contents of the 17 analytes. Sativanone and 3'-
-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 CH
, CO, and CO
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
.
•Thirty-one organophosphorus pesticides residues in Alpinia oxyphylla were determined.•Sample preparation was completed in a single step without any clean-up procedure.•The proposed method was ...successfully applied to 55 commercial samples.•Seven organophosphorus pesticides were detected in eight of the samples.•The positive samples were further confirmed by GC–MS/MS.
A simple, rapid and effective gas chromatography–flame photometric detection method was established for simultaneous multi-component determination of 31 organophosphorus pesticides (OPPs) residues in Alpinia oxyphylla, which is widely consumed as a traditional medicine and food in China. Sample preparation was completed in a single step without any clean-up procedure. All pesticides expressed good linear relationships between 0.004 and 1.0μg/mL with correlation coefficients higher than 0.9973. The method gave satisfactory recoveries for most pesticides. The limits of detection varied from 1 to 10ng/mL, and the limits of quantification (LOQs) were between 4 and 30ng/mL. The proposed method was successfully applied to 55 commercial samples purchased from five different areas. Five pesticide residues were detected in four (7.27%) samples. The positive samples were confirmed by gas chromatography with tandem mass spectrometry (GC–MS/MS).
Morinda officinalis is an important herbal medicine and functional food, and its main constituents include anthraquinone and iridoid glycosides. Quantification of the main compounds is a necessary ...step to understand the quality and therapeutic properties of M. officinalis, but this has not yet been performed based on liquid chromatography/tandem mass spectrometry (LC-MS/MS). Analytes were extracted from M. officinalis by reflux method. Ultrahigh-performance liquid chromatography coupled with a triple quadrupole mass spectrometry (UPLC-QqQ-MS) using multiple reaction monitoring (MRM) mode was applied for quantification. Fragmentation pathways of deacetyl asperulosidic acid and rubiadin were investigated based on UPLC with quadrupole time-of-flight tandem mass spectrometry (Q/TOF-MS) in the MSE centroid mode. The method showed a good linearity over a wide concentration range (R2 ≥ 0.9930). The limits of quantification of six compounds ranged from 2.6 to 27.57 ng/mL. The intra- and inter-day precisions of the investigated components exhibited an RSD within 4.5% with mean recovery rates of 95.32–99.86%. Contents of selected compounds in M. officinalis varied significantly depending on region. The fragmentation pathway of deacetyl asperulosidic and rubiadin was proposed. A selective and sensitive method was developed for determining six target compounds in M. officinalis by UPLC-MS/MS. Furthermore, the proposed method will be helpful for quality control and identification main compounds of M. officinalis.
Mycotoxins can occur naturally in a variety of agriculture products, including cereals, feeds, and Chinese herbal medicines (TCMs), via pre- and post-harvest contamination and are regulated ...worldwide. However, risk mitigation by monitoring for multiple mycotoxins remains a challenge using existing methods due to their complex matrices. A multi-toxin method for 22 mycotoxins (aflatoxin B
, B
, G
, G
, M
, M
; ochratoxin A, B, C; Fumonisin B
, B
, B
; 15-acetyldeoxynivalenol, 3-acetyldeoxynivalenol, diace-toxyscirpenol, HT-2, T-2, deepoxy-deoxynivalenol, deoxynivalenol, neosolaniol, zearalenone, and sterigmatocystin) using centrifugation-assisted solid-phase extraction (SPE) clean-up prior to ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis for Arecae Semen and its processed products was developed and validated. Several experimental parameters affecting the extraction and clean-up efficiency were systematically optimized. The results indicated good linearity in the range of 0.1-1000 μg/kg (
> 0.99), low limits of detection (ranging from 0.04 μg/kg to 1.5 μg/kg), acceptable precisions, and satisfactory recoveries for the selected mycotoxins. The validated method was then applied to investigate mycotoxin contamination levels in
and its processed products. The mycotoxins frequently contaminating
were aflatoxins (AFs), and the average contamination level and number of co-occurring mycotoxins in the Arecae Semen slices (Binlangpian) were higher than those in commercially whole Arecae Semen and Arecae Semen Tostum (Jiaobinlang). Sterigmatocystin was detected in 5 out of 30 Arecae Semen slices. None of the investigated mycotoxins were detected in Arecae pericarpium (Dafupi). The results demonstrated that centrifugation-assisted SPE coupled with UHPLC-MS/MS can be a useful tool for the analysis of multiple mycotoxins in
and its processed products.
Notoginseng Radix et Rhizoma (Sanqi in Chinese) is a precious traditional Chinese herbal medicine. It has the effect of dispersing blood stasis and stopping bleeding, reducing swelling and fixing ...pain. However, it tends to contaminate with harmful fungi during storage, which may make it much less effective. In order to understand the fungal contamination of Notoginseng Radix et Rhizoma and master its composition of the exogenous fungi. The surface fungi of Notoginseng Radix et Rhizoma samples collected from six Chinese provinces and districts were investigated by using dilution plate method. Detection of aflatoxins by UPLC-MS/MS. The results showed that Penicillium citrinum was dominantly isolated from Notoginseng Radix et Rhizoma samples from No.1 to No.4. Aspergillus flavus, which produces aflatoxin, was dominantly isolated from Notoginseng Radix et Rhizoma samples from No.5 and No.6. In addition, kinds of mycotoxin were assayed which were produced by three of those identified A. flavus. All three fungi strains produced aflatoxin B1 (AFB1) and one strain HBSQ1-5 additionally produced other three kinds of mycotoxin, AFB2, AFG1 and AFG2. It is the results implied that it will be very important to take serious cautions when using Notoginseng Radix et Rhizoma. As well as, understanding the composition of the exogenous fungi of Notoginseng Radix et Rhizoma and the strains of toxin-producing fungi, which can play an important role in guiding the storage of Notoginseng Radix et Rhizoma..
Indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) is an ideal immunoassay method for large-scale screenings to detect mycotoxin contaminants. However, the matrix effect of complicated ...samples has always been challenging when performing immunoassays, as it leads to false-positive or negative results. In this study, convenient QuEChERS technology combined with optimizing the dilution solvent was ingeniously used to eliminate interference from the sample matrix to greatly improve the detection accuracy, and reliable ic-ELISAs for the two official tolerance levels of 60 and 500 μg/kg were developed to screen zearalenone (ZEN) in edible and medical coix seeds without any further correction. Then, the 122 batches of coix seeds were determined, and the positive rate was up to 97.54%. The contaminated distribution was further analyzed, and risk assessment was subsequently performed for its edible and medical purposes. The findings indicated that consumption of coix seeds with higher ZEN contamination levels may cause adverse health effects for both medical and edible consumption in the adult population; even under the condition of average contamination level, ZEN from coix seeds was the more prominent contributor to the total risk compared to other sources when used as food; thus, effective prevention and control should be an essential topic in the future.
, a critically endangered tree species, produces heartwood containing a vast variety of flavonoids. This heartwood, also known as Chinese rosewood, has high economic and medicinal value, but its ...formation takes several decades. In this study, we showed that discolored wood induced by pruning displays similar color, structure, and flavonoids content to those of natural heartwood, suggesting that wounding is an efficient method for inducing flavonoid production in
. Transcriptome analysis was performed to investigate the mechanism underlying wounding-induced flavonoids production in
heartwood. Wounding upregulated the expression of 90 unigenes, which covered 19 gene families of the phenylpropanoid and flavonoid pathways, including PAL, C4H, 4CL, CHS, CHI, 6DCS, F3'5'H, F3H, FMO, GT, PMAT, CHOMT, IFS, HI4'OMT, HID, IOMT, I2'H, IFR, and I3'H. Furthermore, 47 upregulated unigenes were mapped to the biosynthesis pathways for five signal molecules (ET, JA, ABA, ROS, and SA). Exogenous application of these signal molecules resulted in the accumulation of flavonoids in cell suspensions of
, supporting their role in wounding-induced flavonoid production. Insights from this study will help develop new methods for rapidly inducing the formation of heartwood with enhanced medicinal value.
In the storage of
Alpinia oxyphylla
, growth of mildew (especially toxic fungi, such as
Aspergillus flavus
) is a potential safety risk. Few reports have investigated how
A. oxyphylla
storage ...conditions impact mold growth or how mold growth impacts the bioactive components of
A. oxyphylla
. In this study, sterilized
A. oxyphylla
samples were contaminated by artificial inoculation of
A. flavus
spores. The main chemical components and aflatoxin levels in the infected
A. oxyphylla
samples were characterized. Central composite design-response surface methodology was used to study the effects of different temperature and humidity of storage conditions on the fungal growth in
A. oxyphylla
and accumulation of aflatoxins. The results showed that aflatoxins levels can be minimized by storing samples at temperatures below 25 °C and with humidity less than 85%. Additionally, we found that the yield and composition of volatile oil in
A. oxyphylla
exhibited small changes due to mold growth. However, polysaccharide content reduced remarkably. Temperatures below 25 °C and humidity below 85% were the best storage conditions to preventing
A. oxyphylla
from becoming moldy. Our results provide the theoretical basis for future studies the effects of storage conditions and mold growth on the quality and safety of traditional Chinese medicines (TCMs).
Plant growth retardants may play an important role in regulation of yield and quality of crops, fruits, and vegetables. Such compounds have begun to be used in the cultivation of traditional Chinese ...medicines (TCMs), especially for root medicines. Although the potential risks to human health of these compounds has attracted increasing attention, analytical methods for detection of plant growth retardants in TCMs remain poorly investigated. In this study, an effective and reliable method for simultaneous determination of 11 plant growth retardants in Ophiopogon japonicus and soil samples was developed by ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-QqQ-MS/MS). Extraction was conducted in acetonitrile containing 1.0% (v/v) acetic acid with ultrasonication. The octadecylsilyl (C18) and MgSO4 were used as the dispersive-solid phase extraction (d-SPE) sorbent and provided satisfactory recoveries for the analytes. The conditions of extraction and LC-MS/MS were optimized to achieve the highest recovery and sensitivity. Good linearity was achieved within a wide range with all correlation coefficients exceeding 0.9950. The recoveries of all analytes in O. japonicus and soil samples ranged from 57.37% (choline chloride) to 99.93% (trinexapac-ethyl) and from 54.37% (daminozide) to 94.82% (triadimenol), respectively. The limits of quantifications ranged from 0.03 to 3.54 μg/L. The proposed method was successfully applied to detect and quantify 11 plant growth retardants in empirical O. japonicus and soil samples. High frequency of paclobutrazol and choline chloride was found in O. japonicus samples. In addition, paclobutrazol showed a high residual concentration (>1100 μg/kg) in the soil of O. japonicus indigenous production.
A multi-residue method was proposed for simultaneous analysis of 11 plant growth retardants in Ophiopogon japonicus by using d-SPE and UPLC-MS/MS. Display omitted
•A versatile UPLC-MS/MS analytic method for 11 plant growth retardants is proposed.•Octadecylsilyl and magnesium sulfate anhydrous were used as the d-SPE sorbent.•Paclobutrazol and choline chloride were detected at high frequency in O. japonicus.•Residual level of paclobutrazol in O. japonicus planted soil was high.
•QuEChERS-dSPE-UPLC-MS/MS method was developed for 21 mycotoxins.•Quantification was made by matrix-matched combined with internal standard.•Validation data were consistent with European Commission ...guideline requirements.•Aflatoxins were detected in nutmeg.•The proposed method is effective for the determination of multi-mycotoxins.
Nutmeg (Myristica fragrans), a popular spice and traditional medicine worldwide, is susceptible to fungal and mycotoxin contamination. Hence, it is important to monitor the residual levels of multiple mycotoxins in nutmeg and related products. However, analysts are continuously faced with the challenges of quantifying mycotoxin concentrations in complex matrices such as spices and traditional Chinese medicines. To develop a simple and sensitive mycotoxin analysis method encompassing the total workflow from sample preparation to quantitative analysis, a simple, robust, and sensitive method for the simultaneous identification and quantification of 21 mycotoxins in nutmeg and related products was described. The method is based on sample preparation by modified QuEChERS extraction and dispersive solid-phase extraction (dSPE) cleanup followed by ultrahigh-performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS). Matrix-matched calibration was applied for the quantification of the investigated mycotoxins. The limits of detection of the target analytes ranged from 0.04 μg/kg to 6.0 μg/kg. Recovery rates ranged from 60.49% to 97.46% at three spiking levels, with relative standard deviations<13%. This method was applied to 45 samples of nutmegs, mace and related products. Three nutmeg samples and one nutmeg powder were contaminated with aflatoxins with residue levels of 1.76 ~ 3.39 μg/kg for AFB1 and 2.51 ~ 8.77 μg/kg for AFs (the sum of AFB1, AFB2, AFG1, AFG2 and AFM1). No mycotoxins were detected in mace. All of the contamination levels were below the regulatory maximum residue limits suggested by the European Commission and China.
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