最新刊期
卷 41 ， 期 6 ， 2022
- 摘要：An ultra-high performance liquid chromatography－quadrupole/electrostatic field orbitrap high resolution mass spectrometry（UPLC－Q/Orbitrap HRMS） was established for the non-targeted screening of phenylurea herbicides and benzoylurea insecticides in apples. Apple samples were extracted with acetonitrile，then purified by QuEChERS method. The purified solution was separated on an Acquity BEH C18 column（100 mm × 2.1 mm，1.7 µm） using a gradient mobile phase consisting of water（containing 0.1% formic acid ） and methanol，then analyzed by HRMS with electrospray ion source under positive ion mode. The 13 phenylurea herbicides and 9 benzoylurea insecticides were divided into four groups based on their structural differences. The secondary mass fragments of four typical standards in the four groups of phenylurea herbicides and benzoylurea insecticides were analyzed，and then，the regularities of the characteristic fragment ions and neutral loss fragments produced by collision induced dissociation of the phenylurea herbicides and benzoylurea insecticides were summarized. The main characteristic fragment ions of 9 herbicides such as chlorotoluron are m/z 72.044 59，and fragments can also be produced by neutral loss of dimethylamine（m/z 45.058 03）. Four herbicides such as monolinuron lose neutral methanol ［CH3OH］ m/z 23.025 59 or hydrogen halide ［HR1］（R=Cl，Br，F）to produce fragment ions.The main characteristic fragment ions of seven fluorine atom substituted benzoylurea insecticides such as diflubenzuron are m/z 158.040 47 and m/z 141.015 00，and the neutral loss of 2，6-fluorobenzamide structure［C8H3F2O2NH2］（m/z 183.013 21） can produce characteristic fragment ions. The main characteristic fragment ions of triflumuron and chlorobenzuron，which were chlorine atom substituted benzoylurea insecticides，are m/z 156.020 25，m/z 138.993 76 and m/z 113.015 28. A total of 12 apple samples collected from local supermarket in Beijing were screened by this non-targeted method. Chlorotoluron was identified and confirmed in one apple sample，which demonstrated that the method could achieve rapid and accurate non-targeted screening of phenylurea pesticides in apples. The proposed mass spectrometry fragmentation pathway in this study provides an important basis for the rapid identification and analysis of phenylurea and benzoylurea compounds with similar structural characteristics in complex systems.关键词：phenylurea herbicides;benzoylurea insecticides;electrostatic field orbitrap high resolution mass spectrometry;fragmentation pathway;non-targeted screening
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发布时间：2022-06-22 - 摘要：A novel ultra-performance liquid chromatography - tandem mass spectrometry（UPLC - MS/MS） with polystyrene（PS） nanofiber solid phase extraction was developed for the simultaneous determination of 25 glucocorticoids in milk after the optimization of chromatographic and extraction conditions. The PS nanofiber was prepared by electrostatic spinning，then characterized by scanning electron microscopy， transmission electron microscopy and infrared spectroscopy. Subsequently， the BET surface area and contact angle of the PS nanofiber were measured. The milk sample was extracted using vortex mixer with acetonitrile. The analytes were concentrated and purified with the PS nanofiber solid phase extraction column. The chromatographic separation of the methanol eluent was performed on an ACQUITY BEH C18 （2.1 mm × 100 mm，1.7 μm） column by gradient elution，with 0.1% formic acid aqueous solution and acetonitrile as mobile phases. The analysis was performed by mass spectrometry with jet stream electrospray ionization in positive mode under multiple reaction monitoring（MRM） mode. The analytes were quantified by external standard method. Results of the method validation showed that there were good linear relationships for 25 glucocorticoids in the concentration range of 1 - 100 µg/L，with their correlation coefficients（r） larger than 0.995.The limits of detection（LOD，S/N ≥ 3） and limits of quantitation（LOQ，S/N ≥ 10） for 25 glucocorticoids were in the range of 0.04 - 0.10 µg/kg and 0.13 - 0.33 μg/kg，respectively. The recoveries for 25 glucocorticoids in the spiked sample at three concentration levels ranged from 71.5% to 105%，with relative standard deviations（RSDs） of 1.8% - 10%. The established method is simple，rapid，accurate and sensitive. The method was applied to detect 25 glucocorticoids in 10 batches of milk samples. Only one of them were found to contain trace hydrocortisone residue.关键词：glucocorticoids;nanofiber solid phase extraction;polystyrene;ultra-performance liquid chromatography - tandem mass spectrometry;milk
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发布时间：2022-06-22 - 摘要：A liquid chromatography－quadrupole-time-of-flight mass spectrometry（LC－Q－TOF MS） with a modified QuEChERS method was developed for the detection of 33 pesticide residues，including 8 neonicotinoid insecticides and 25 fungicides in four tropical fruits（mango，banana，sweetsop and wax apple）．The pretreatment parameters were optimized by comparing the spiked recoveries obtained with different extraction solvent volumes，buffer salts，and clean-up adsorbent types．Under the optimal experimental conditions，the tropical fruit samples were extracted with 1% acetonitrile acetate in buffer salts（EN salts），and subsequently purified in 15 mL tubes of 900 mg MgSO4，150 mg PSA，50 mg C18 and 15 mg GCB．The sample solutions were detected by LC－Q－TOF MS in positive ion mode under all-ion fragmentation acquisition mode（All Ions MS/MS），and quantified by the matrix-matched external standard method．The method could effectively reduce the matrix effect．Under the optimized conditions，the 33 pesticides showed good linearity in their respective linear ranges，with their correlation coefficients（r2） more than 0.99．The screening detection limits（SDLs） for four tropical fruits were in the range of 0.5－20 µg/kg，and the limits of quantitation（LOQs） were in the range of 0.5－50 µg/kg．The accuracy and precision of the method were verified by the spiked recovery experiments for mangoes．The recoveries for 33 pesticides at three spiked levels ranged from 70.5% to 116%，with relative standard deviations（RSDs） no more than 20%．Meanwhile，the method was successfully applied to the detection of 102 commercial tropical fruits samples．Characterized with simplicity，rapidness and sensitivity，the method was suitable for the detection of neonicotinoid pesticide and fungicide residues in tropical fruits．关键词：tropical fruits;liquid chromatography－quadrupole-time-of-flight mass spectrometry （LC－Q－TOF MS）;QuEChERS;neonicotinoid insecticides;fungicides
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发布时间：2022-06-22 - 摘要：A gas chromatography－tandem mass spectrometric（GC－MS/MS） method was developed for the rapid determination of 75 pesticide residues in codonopsis radix，based on modified dispersive solid phase extraction using hydroxylated multi-walled carbon nanotubes（MWCNTs－OH） as sorbent．The samples were extracted with ethyl acetate，then salted out and cleaned up with anhydrous magnesium sulfate，sodium acetate，N-primary secondary amine（PSA） and MWCNTs－OH，finally analyzed by gas chromatography－tandem mass spectrometry in the dynamic multiple reaction monitoring（dMRM） mode and quantified by the matrix-matched external standard method．There were good linear relationships for 75 pesticides in the range of 5－300 μg/L，with correlation coefficients（r2） no less than 0.996 1．The limits of detection（LODs） and the limits of quantitation（LOQs）were 0.001－0.054 mg/kg and 0.002－0.178 mg/kg，respectively．The average recoveries at four spiked levels of 0.025，0.05，0.20 and 0.50 mg/kg ranged from 69.7% to 113%，with relative standard deviations（RSDs，n = 4） of 0.64%－6.7%．This method is simple，rapid and accurate，and it is suitable for high-throughput detection of pesticide residues in codonopsis radix．关键词：hydroxylated multi-walled carbon nanotubes;dispersive solid phase extraction;gas chromatography－tandem mass spectrometry;pesticide residues;codonopsis radix
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发布时间：2022-06-22 - 摘要：A high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） with QuEChERS pretreatment was developed for the simultaneous determination of six teicoplanins in fish samples．The six components in minced fish samples were extracted with acetonitrile－10% trichloroacetic acid（6∶4） mixed solution．Then the extracted supernatant was cleaned up with 100 mg of primary secondary amine（PSA）．Separation of the targets was performed on an Agilent SB C18 chromatographic column（2.1 mm × 100 mm，1.8 µm） by gradient elution，using 0.1% formic acetonitrile and 0.1% formic as the mobile phase A and the mobile phase B，respectively．The six targets were detected in positive ion electrospray ionization mode（ESI+） under multiple reaction monitoring（MRM） mode，then quantified by the internal standard method with polymyxin sulfate B as the internal standard（IS）．Effects of different types and volumes of extraction solvent，different types and dosages of adsorbent on recoveries of six targets were investigated in detail．The matrix effects of six teicoplanins in different fish substrates were evaluated by the ratio of solvent standard curve and matrix-matched standard curve．Under the optimal conditions，six teicoplanins were well separated by HPLC－MS/MS within 4 min．Good linear relationships were obtained for six analytes in the concentration range of 1－100 μg/L，with their correlation coefficients（r2） greater than 0.998．At three spiked levels of 5.0，10.0 and 25.0 μg/kg，the average recoveries for six analytes in different fish samples ranged from 84.3% to 93.3%，with intra-day relative standard deviations（intra－RSDs） and inter-day relative standard deviations（inter－RSDs） not more than 7.0% and 6.2%，respectively．The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 0.5－2.0 μg/kg and 2.0－5.0 μg/kg，respectively. The established method was applied to the detection of teicoplanins in various fish samples（forty fish samples that were divided into nine varieties，containing carp，crucian，grass carp，chub，silver carp，mandarin fish，tilapia，pseudosciaena crocea，and scophthalmus maximus） by random sampling principle，and no component of teicoplanin was detected in these actual samples．The developed method proved to be simple，sensitive，accurate and reliable，and was suitable for the simultaneous determination of six teicoplanins in fish samples.关键词：teicoplanins;QuEChERS;high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）;fish samples
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发布时间：2022-06-22 - 摘要：A method was established for the determination of 17 parabens in fruits by ultra performance liquid chromatography－quadrupole electrostatic field orbitrap high-resolution mass spectrometry（UPLC－Q－Orbitrap HRMS）．The samples were ultrasonically extracted with methanol．Data was acquisited with electrospray ionization（ESI） ion sources in negative ion mode．The chromatographic conditions，MS conditions，types and amounts of extraction solvents were optimized，and the cracking mechanisms and matrix effects of the compounds were analyzed．The matrix curves for 17 parabens showed good linear relationships in the range of 2－200 μg/L，with correlation coefficients（r2） not less than 0.997 5．The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 5－30 μg/kg and 20－100 μg/kg，respectively．The average spiked recoveries ranged from 70.7% to 117%，with relative standard deviations（RSDs） of 1.5%－4.8%．The method was simple，efficient and operable，and could satisfy the requirements for the rapid determination of parabens in fruits．关键词：ultra performance liquid chromatography－quadrupole electrostatic field orbitrap high-resolution mass spectrometry（UPLC－Q－Orbitrap HRMS）;fruit;parabens;rapid determination
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发布时间：2022-06-22 - 摘要：An ultra performance liquid chromatography（UPLC） coupled with evaporative light scattering detection（ELSD） was established for the determination of 12 saccharides，i.e．fructose，glucose，sucrose，turanose，mlatulose，maltose，kojibiose，isomaltose，erlose，melezitose，raffinose and maltotriose in honey. Honey sample was dissolved in deionized water and kept constant volume with acetonitrile．The solution was then filtered with a 0.22 μm filter membrane．12 saccharides were separated on an Amide column，then determined with an evaporative light scattering detector，and finally quantified by external standard calibration method．Through the optimization experiment，there existed good linear relationships for 12 saccharides，and the linear correlation coefficients were in the range of 0.997 7－0.999 8．The obtained results for fructose and glucose by this method were comparable to those of the traditional refractive index detection method．The average recoveries for the other 10 saccharides ranged from 90.0% to 105%，and the relative standard deviations were between 0.70% and 5.8%．The method was validated to be sensitive，accurate and repeatable．It was suitable for simultaneous quantitative analysis of multiple sugar components in honey．The proposed method was applied to the determination of 12 saccharides in 72 batches of honey samples of different botanical origins．It was found that turanose，mlatulose and maltose are the dominant disaccharides in Chinese honeys．This method and test data provided an important support for honey quality and quality evaluation．关键词：honey;sugar;high performance liquid chromatography;evaporative light scattering detection
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发布时间：2022-06-22 - 摘要：A gas chromatography－mass spectrometric（GC－MS） method was established for the analysis of novel synthetic indazoles cannabinoids in“E－cigarette oil”．The samples were extracted with methanol．With diazepam as internal standard，9 novel synthetic cannabinoids were then determined with an HP－5MS column（30 m × 0.25 mm × 0.25 μm） and quantified by internal standard method under such programmed temperature conditions，namely，setting the initial temperature at 200 ℃ for 1 min，then increasing the temperature to 260 ℃ at a rate of 20 ℃/min and keeping for 1 min，and finally increasing the temperature to 300 ℃ at a rate of 5 ℃/min and kept for 10 min．Meanwhile，the mass spectrum of the target fragment fracture manner was analyzed．9 target substances could be effectively separated in 20 min．And the correlation coefficients（r2） were all greater than 0.997 in the linear range of 1.0－100.0 µg/mL．The detection limits and quantitation limits were in the ranges of 0.04－0.25 μg/mL and 0.15－0.85 μg/mL， respectively．The recoveries ranged from 95.1% to 104%，with intra-day relative standard deviations（RSDs） and inter-day RSDs less than 4.6% and 8.4%，respectively．The results showed that the method is effective，accurate and sensitive，and it could be applied to the analysis for actual cases.关键词：gas chromatography－mass spectrometry;E－cigarette oil;indazoles synthetic cannabinoid
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发布时间：2022-06-22 - 摘要：A method was developed for the determination of the migration amounts of 5 compounds，i.e.aniline，N-methylaniline，1，3-diphenylguanidine，2-mercaptobenzothiazole and benzothiazole in food contact rubber liners by high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）．The separation of target compounds was performed with an Agilent Poroshell 120EC－C18 column（3 mm × 50 mm，2.7 μm），using 0.1%（volume fraction） formic acid and acetonitrile solution as mobile phases by gradient elution．The detection on the analytes was performed with positive electrospray ionization source under multiple reaction monitoring（MRM） mode，and the quantitation was carried out by the external standard method．Under the optimized conditions，the calibration curves were linear in the respective mass concentration ranges，with correlation coefficients（r2） not less than 0.996 6．The limits of detection（LODs，S/N = 3） and quantitation（LOQs，S/N = 10） were in the ranges of 0.8－20 μg/L and 3－50 μg/L，respectively．The average recoveries for 5 compounds at the spiked levels of 3－500 μg/L were in the range of 93.4%－112%，with relative standard deviations（RSDs） of 0.70%－4.3%．This method was used to detect the migration amounts of 5 compounds in 10 kinds of food contact rubber liners under the three conditions（40 ℃ for 10 min，40 ℃ for 30 min and 40 ℃ for 120 min）．According to the migration results，5 compounds in all liners were detected，and the migration amounts of 1，3-diphenylguanidine and 2-mercaptobenzothiazole were within the limit range．The detection of benzothiazole needs attention．The migration amounts of aniline and N-methylaniline were higher than its migration limit（0.01 mg/kg），and the generation of aniline and N-methylaniline must be controlled by improving the formulation or the process．This method has the advantages of simple operation and high sensitivity，and it is suitable for the determination of 5 compounds in food contact rubber liners．关键词：food contact rubber liners;high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）;food simulants;migration
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发布时间：2022-06-22 - 摘要：A headspace gas chromatography－mass spectrometry（HS/GC－MS） with chemometrics was developed for analysis of the main volatile substances in three raw paperboards and three metallic ink-printed paperboard samples．The volatile substances in sample fragments were analyzed by HS/GC－MS，followed by MS－DIAL deconvolution，NIST mass library and retention index match．Meanwhile，the relative contents of peaks as well as the relative odour active values（ROAV） were calculated to analyze the key odour substances and their impacts．The results obtained showed that，a total of 63 volatile compounds were detected in all paperboard samples，of which 46 volatile compounds were identified，mainly including aldehyde，ketones，alkane and alkene substances．More aldehydes and ketones compounds were found in the paperboard samples printed with different metallic inks，affecting the overall sensory evaluation．19 key odour substances were selected，including benzenaldehyde，n-octanaldehyde，（E，E）-2，4-hepadienaldehyde，n-decanol，2-amylfuran，and their models of principal component analysis（PCA），orthogonal partial least squares discriminant analysis（OPLS－DA） and hierarchical cluster analysis（HCA） were established，showing that the key odour substances（ROAV > 10） had unconspicuous effect and distributed in different raw paperboards and the metallic ink-printed products．关键词：headspace gas chromatography－mass spectrometry;multivariate statistical analysis;metallic ink;volatile substances;odour
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发布时间：2022-06-22
Scientific Papers
- 摘要：It is of great significance to develop novel analysis techniques for simultaneous determination of dapsone and its metabolites in aquatic products，so as to realize the simultaneous supervision of dapsone and its metabolites in aquatic products and the comprehensive control of illegal drug use．In this study，a high performance liquid chromatography－tandem triple quadrupole mass spectrometric（HPLC－MS/MS） method was established for the determination of dapsone and its metabolite residues in aquatic products．In the process of sample pre-treatment，the samples were extracted by using 10 mL 1% ammoniated acetonitrile with dapsone-D8 as the internal standard，followed by fat removal with n-hexane．Meanwhile，MCX cationic solid phase extraction column was used for enrichment and purification．The eluent was concentrated to about 0.2 mL by nitrogen blowing at 45 ℃，and then fixed with 10% methanol solution to 1 mL．After mixing，the eluent was filtered through a 0.22 μm aqueous phase membrane into an injection vial for detection by HPLC－MS/MS．The separation was carried out on a CAPCELL PAK C18（2.0 mm × 100 mm，3 µm） by gradient elution using methanol－water as mobile phases．The quantitative analysis of target compounds was performed by the internal standard method under multiple reaction monitoring（MRM） and positive ion ionization modes．The results showed that the calibration curves for dapsone and N-acetyl dapsone were linear in the mass concentration range of 0.1－5.0 μg/kg，with correlation coefficients（r2） all greater than 0.99．The limits of detection（LODs） were 0.1 μg/kg and the limits of quantitation（LOQs） were 0.2 μg/kg．The average recoveries at three spiked levels of 0.2，1.0，2.0 μg/kg ranged from 94.0% to 109%，with relative standard deviations（RSDs） of 2.7%－11%．The positive muscle samples obtained in the drug substitution experiment were determined，and the metabolite of dapsone was identified as N-acetyl dapsone by identifying the retention time of the compound and the ion pair information．This method has low detection limit，good precision and high accuracy，which could realize the accurate qualitative and quantitative determination of dapsone residues in fish，shrimp，crab，shellfish and other aquatic products．关键词：high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）;dapsone;N-acetyl dapsone;MCX solid phase extraction;aquatic products
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发布时间：2022-06-22 - 摘要：An high performace liquid chromatography－tandem mass spectrometric method was established for determination of the specific migration of five fluorescent whitening agents，i.e FWA184，FWA185，FWA393，FWA367 and FWA135 in food processing machinery material sealing rubber washer．The migration law for 5 fluorescent whitening agents transferring from food processing machinery material sealing rubber washer into 4 food simulants（water，4% acetic acid，50% ethanol and olive oil） was investigated．The results showed that there were good linear relationships for five fluorescent whitening agents in the concentration range of 5－100 μg/L，with their correlation coefficients（r） not less than 0.999 1．The limits of quantitation（LOQ） of the method were 0.001－0.050 mg/kg．In olive oil，the average recoveries at three spiked levels of 0.05，0.1， 0.5 mg/kg ranged from 81.8%－101%，with relative standard deviations（RSDs，n＝10） of 1.2%－5.6%. As proved，this method was simple and fast，which satisfies the requirements（including sensitivity，specificity and selectivity） for determining fluorescent whitening agents in food processing machinery material sealing rubber washer．Under the same conditions，the migration of 5 fluorescent whitening agents in sealing rubber washer was the highest in olive oil．With the increase of temperature，the migration of 5 fluorescent whitening agents increased significantly，while with the extension of contact time，the migration of 5 fluorescent whitening agents showed a process from rapid migration to slow migration，and then tended to reach an equilibrium．关键词：sealing rubber washer;fluorescent whitening agents;high performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）;food simulants;migration law
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发布时间：2022-06-22 - 摘要：Cross-linked porcine liver esterase hybrid“nanoflower”enzyme（CL－PLE－NF） was prepared via biomineralization coupling wet cross-linking，and the preparation conditions were optimized. Under the optimum conditions，the activity and maximum reaction rate of CL－PLE－NFs exhibited 231% and 134% those of free enzyme，respectively．After stored at 4 ℃ for 320 days，the CL－PLE－NFs still retained 70.85% of initial activity，which indicates its good storage stability．Additionally，pyrethroid pesticides were employed to investigate the hydrolysis performance of CL－PLE－NFs．It was found that eleven kinds of pyrethroid pesticides，including type Ⅰ and type Ⅱ，gave over 55% hydrolysis efficiency in 5 min．After 12 cycles of use，the hydrolysis efficiency of Cl－PLE－NFs for detamethrin still maintained 65.37%．关键词：glutaraldehyde;cross-linking;pyrethroid pesticide;digestion;storage stability;reusability
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发布时间：2022-06-22 - 摘要：In order to assess the risks from the migration of additives in food contact plastics，a method for simultaneous determination of the migration of 50 additives in food contact plastics was established by ultra-performance liquid chromatography－quadrupole time-of-flight mass spectrometry（UPLC－QTOF MS）．Methanol and the aqueous mixture of formic acid（0.01%，volume fraction） and 5 mmol/L ammonium acetate were adopted as the mobile phases for elution．The primary and secondary ions of the target were monitored in target ion acquisition（Target MS/MS） mode．The results of each substance showed good linear relationships in the mass concentration range of 0.02－5 mg/L．The detection limits of the method were between 0.01 mg/kg and 0.1 mg/kg，and the spiked recoveries ranged from 92.6% to 104%，with the relative standard deviations（RSDs） of 0.60%－8.4%．A total of 12 plastic samples were detected in 20 actual samples，of which nonylphenol was detected in 2 samples，and the migration amounts were 0.033－0.071 mg/kg．Meanwhile，antioxidant 1076 and antioxidant 168 were found in 6 samples，and the migration amounts ranged between 0.12 mg/kg and 3.3 mg/kg，while photoinitiator 369，photoinitiator ITX and photoinitiator TPO were detected in 4 samples，and the migration amounts were between 0.054 mg/kg and 4.0 mg/kg. The method is sensitive，accurate and simple，and it is suitable for the detection of migration of 50 additives in plastics for food contact materials.关键词：plastic additives;migration;food contact materials;ultra-performance liquid chromatography－quadrupole time-of-flight mass spectrometry
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发布时间：2022-06-22 - 摘要：An analytical method was established for the determination of 12 antioxidants in medicinal rubber plugs by ultra performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）．The rubber plug sample was soaked with 20% ethanol for 72 h at 60 ℃．The extracting solution was extracted by acetonitrile assisted salting-out liquid extraction，followed by clean-up through a 0.22 μm PTFE membrane．The separation was conducted on a Hypersil Gold C8 chromatographic column（100 mm × 2.1 mm，1.9 μm） with methanol－water（containing 0.02% formic acid and 5 mmol/L ammonium formate） as mobile phase．The target compounds were detected in turn under electrospray ionization（ESI） positive and negative ion multiple reactive monitoring（MRM） mode，and quantified by external standard method．The results showed that under the optimized conditions，12 antioxidants exhibited good linearity，with correlation coefficients（r2） all greater than 0.995. The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 0.10－25 ng/g and 0.25－75 ng/g，respectively．The average recoveries ranged from 75.6% to 117%，with the relative standard deviations（RSDs，n = 6） of 0.90%－8.4%．With the advantages of simple pretreatment，high accuracy，low detection limit and short analysis time（6 min），this method could be used for the rapid screening of 12 antioxidants in medicinal rubber plugs．关键词：antioxidants;UPLC－MS/MS;medicinal rubber plugs
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发布时间：2022-06-22 - 摘要：A gas chromatography－tandem mass spectrometric（GC－MS/MS） method was established for the simultaneous detection of 10 N-nitrosamines including N-nitrosodimethylamine in cosmetics. After pretreated by QuEChERS method，the samples were extracted with acetonitrile，then purified by enhanced lipid removal products（EMR－Lipid dSPE）. The analytes were separated on a polyethylene glycol quartz column HP－INNOWAX（30 m × 0.25 mm × 0.25 µm），then analyzed in multiple reaction monitoring（MRM） mode，and finally quantified by the external standard method. There were good linear relationships for the 10 N-nitrosamines in the range of 0.5－50 ng/mL，with their correlation coefficients（r） larger than 0.999. The limits of detection and limits of quantitation were 1 µg/kg and 3 µg/kg，respectively. The average recoveries for 10 N-nitrosamines at the spiked levels of 5， 50，200 µg/kg ranged from 80.5% to 143%，with the relative standard deviations（RSDs） less than 11%（n = 6）. The developed method was simple，rapid，exclusive，sensitive，accurate and precise，and it could be applied in the rapid determination of 10 N-nitrosamines in cosmetics.关键词：gas chromatography－tandem mass spectrometry;QuEChERS;cosmetics;N-nitrosamines
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发布时间：2022-06-22
Experimental Techniques and Methods
- 摘要：The quality and safety of consumer products are closely related to people's living standards and socioeconomic development．The improvement of the quality of consumer products is of great significance to promoting the development of consumer product industries，improving domestic consumption environment，and boosting consumer confidence．In recent years，with the continual applications of new materials，formulations and techniques，the categories of consumer products have been greatly broadened，contributing to the improvement of consumers'living quality．However，the accompanying quality and safety issues also put forward higher requirements and challenges for consumer product detection technology．Traditional detection methods，complicated in sample preparation，long in detection period and relying on large-scale instruments，could no longer meet the needs of current economic and social development. Therefore，rapid detection technology has become a key research direction. In this paper，the research progress on rapid detection technology for consumer products in the past five years was reviewed．The present situation and future prospect were discussed，which may provide a useful guidance for relevant researchers and practitioners.关键词：consumer products;rapid detection;research progress;review
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发布时间：2022-06-22 - 摘要：Perfluoroalkyl and polyfluoroalkyl substances（PFAS） are widely used in industrial production and daily life．PFAS have been widely studied and consequently been detected in various environmental and biological matrices around the world due to their potential threats to humans and the environment．The development trend of relevant regulations is to manage PFAS as a chemical class. To date，mass spectrometry（MS） has been a traditional technique for PFAS analysis，among which the low-resolution MS is only limited for target analysis，while high-resolution MS with advantages of high resolution and high mass accuracy，could realize the high throughput analysis for both targets and non-targets at the same time，so as to meet and respond to the requirements for continuous updating and stricter of regulations．The research progress on high-resolution MS in PFAS analysis，including related pretreatment methods are reviewed in this paper．Furthermore，the applications of high-resolution MS in environmental samples，food，consumer goods，human samples and other matrix are also introduced，and the process of non-targeted analysis is described．Finally，knowledge gaps and future perspectives are identified．关键词：perfluoroalkyl and polyfluoroalkyl substances（PFAS）;high-resolution mass spectrometry;review
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发布时间：2022-06-22 - 摘要：Cleaning products are daily used products by consumers．Their quality and safety have drawn considerable concerns by consumers．The hazardous chemical substances potentially existed in cleaning products may pose adverse impacts on the health and safety of consumers．In order to reduce and avoid the quality and safety problems，researchers have utilized a variety of analytical techniques to develop novel analytical methods for the detection of hazardous chemical substances in cleaning products．The research progress on analytical techniques for the quality and safety of cleaning products in recent years is reviewed in this paper，which is anticipating to provide a certain theoretical support or technical guidance for relevant researchers．关键词：cleaning products;quality and safety;analytical techniques;review
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发布时间：2022-06-22 - 摘要：Mouthing behavior is essential and important in the growth and development of children．Children may touch or place all those objects in contact with their mouths when they play or use baby products，thus leading to potential mechanical or chemical risks．At present，most of the chemical safety regulations and standards for toys and baby products worldwide are based on the safety risks assessed through mouthing exposure pathways．Herein，both home and abroad related researches on children’s mouthing contacts with objects are investigated thoroughly，and several aspects are emphasized．The research methods for collecting children’s mouthing behavior parameters are overviewed，and the mouthing behavior parameters of children are reviewed and summarized in terms of contact duration，contact frequency，bite force，mouth size and saliva composition，etc．The deficiencies in investigation on the parameters of children’s mouth based on the safety risk assessment of toy and baby products are analyzed，and finally，the development direction of the research on the exposure behavior and exposure risk based on toys and baby products is proposed．This investigation provides references for mouthing exposure risk assessment，detection and related standardization formulation of toy and baby products．关键词：children mouthing behavior parameter;toy and baby products;safety risk;advance
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发布时间：2022-06-22
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