RSC Advances
·
2022
·Vol. 12
·期 15
·9256-9262
·
IF 4.036
Mengmeng Zhao,Xiaoxia Wu,Zengda Yu,Yunkai Sun,Zhao Liu,Jinqiao Yuan,Hu Liu,Yiping Jin
Avanafil is a phosphodiesterase type 5 inhibitor which is used to treat erectile dysfunction in men. The process-related impurities of avanafil were investigated, and four kinds of impurities in several laboratory batches with a content of 0.29–1.63% were detected by the newly developed gradient ultra-high performance liquid chromatography (UPLC). Based on the synthesis route and UPLC-MS research, the impurities are inferred as Imp-A, Imp-B, Imp-C and Imp-D. The structures of the impurities were inferred from LC-MS studies and confirmed by synthesis, followed by spectroscopic characterization such as NMR and mass spectrometry. Especially, the synthesis of Imp-D is firstly reported. The drug-related substances can be separated well by efficient and selective ultra-high performance liquid chromatography on a Waters ACQUITY HSS C18 (50 × 2.1 mm, particle size 1.8 μm) column at 35 °C, with the mobile phase consisting of ammonium formate (20 mM) and acetonitrile, and the detection at 239 nm with a DAD detector. The method was validated in terms of specificity, linearity, precision, accuracy and sensitivity, and satisfactory results were obtained. The results indicated this developed UPLC method for avanafil and the proposed synthesis mechanism can be used for quality control purposes as required by regulatory agencies to ensure the safety and efficacy of the product.
研究领域:
药物化学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food Analytical Methods
·
2018
·Vol. 11
·期 11
·3170-3178
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IF 2.245
Wang Liao,Chen Yisheng,Ye Zhiyang,Hellmann Bernhard,Xu Xueming,Jin Zhengyu,Ma Qinqin,Yang Na,Wu Fengfeng,Jin Yamei
The cytotoxicity of phenolic antioxidants had attracted marked attention, posing serious challenges to food safety. This paper presented a screening method for two major phenolic antioxidants (butylated hydroxytoluene and tert -butylhydroquinone) added in edible oils. To specifically visualize the targeted compounds after developing with toluene/ethyl acetate/methanol 8:1:1 ( v / v / v ) to 70 mm solvent front, the plate was subjected to a standardized 1,1-diphenyl-2-picrylhydrazyl assay. In addition to synoptical eye inspection, accurate quantification was realized by modified densitometric measurements: fluorescence mode, excitation wavelength 530 nm (D 2 and W lamp) without optical filter, which offered satisfactory sensitivity (8.5–17.5 mg/kg) and acceptable linearity ( R 2 > 0.999 within 50–200 ng/zone). Moreover, the established method was validated with edible oil samples, against EU Directive 2006/52/EC. Apart from that, the unambiguous confirmation of positive results was conveniently achieved by TLC-MS interface-mediated mass spectrometry. Featuring the merits of screening conception, the proposed method not only reached the goal of accurate quantification and conclusive identification of multi-phenolic antioxidants, but also excellently balanced the simplicity, detectability, and throughput of the screening workup. Therefore, it might be an attractive alternative to conventional methods.
研究领域:
食品安全
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分析化学
·
营养学
✓ 已验证
产品关联
DOI
高影响因子
SENSORS AND ACTUATORS B-CHEMICAL
·
2014
·
IF 3.84
Xi Dai,Tao Zhang,Yi-Zhi Liu,Tao Yan,Yun Li,Jun-Ying Miao,Bao-Xiang Zhao
A ratiometric fluorescent probe DPCA based on coumarin and pyrazoline was designed and synthesized for sensing cysteine (Cys) in physiological pH. The probe can detect Cys by fluorescent spectrometry within 40 min with a detection limit of 5.08 μM. The mechanism of DPCA sensing Cys involved conjugate addition/cyclization which was confirmed by HRMS and fluorescence spectra analysis. Moreover, DPCA was able to be applied to complicated conditions with negligible interference from these species and successfully applied in cell imaging.
研究领域:
生物化学
·
细胞生物学
✓ 已验证
DOI
高影响因子
Analytical Methods
·
2014
·Vol. 7
·期 4
·1630-1634
·
IF 1.938
Chunhua Lv,Jiannan Sun,Heyong Cheng
In this work, we report a rapid analytical method for the determination of trace formaldehyde in cosmetics on a 12.5 mm C18 guard column. The shortest time (0.5 min) was obtained for one separation with 1.5 mL min−1 of methanol–water 50 : 50 (v/v) as the mobile phase at a column temperature of 30 °C. A linear response between peak area and the concentration of formaldehyde was obtained over the range 0.1 to 20 mg L−1 with a relative standard deviation of 1.4% (n = 10) at the concentration of 1.0 mg L−1 and a detection limit of 5.1 μg L−1. The confirmation assay by liquid chromatography tandem mass spectrometry indicated that there was no interfering effect from other carbonyl compounds. The proposed method was applied for the determination of formaldehyde residue in cosmetics at the mg L−1 level. Free formaldehyde up to 27 mg kg−1 was found in cosmetics and the spike recovery at the spiked levels of 1.0 and 10.0 mg L−1 varying from 92% to 105% was also obtained. The difference between the values determined by the proposed method and the standard spectrophotometric method was below 3.7%. The results proved the accuracy and precision of the method, showing potential for the routine analysis of formaldehyde residue.
研究领域:
分析化学
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化妆品科学
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
EUROPEAN JOURNAL OF MASS SPECTROMETRY
·
2019
·
IF 0.851
Shencong Lv,Henghui Wang,Yong Yan,Miaohua Ge,Jian Guan
A simple, rapid, and efficient liquid chromatography tandem mass spectrometry (LC–MS/MS) method, operated in electrospray ionization and quadrupole linear ion trap modes, has been developed for the identification and structural characterization of aflatoxins in peanuts and its derivative products or bean sauce. Samples (5 g) were extracted with acetonitrile/water/formic acid (79:20:1, v/v). After centrifugation and dilution, the extracts were separated on a C18 analytical column by gradient elution (acetonitrile/0.2% formic acid) and analyzed by UPLC–MS/MS. External calibration was used for qualification. The developed multiple reaction monitoring–information-dependent acquisition–enhanced product ion method enabled quantification and confirmation of the analytes in a single run. Enhanced product ion mode was used for qualitative analysis, while multiple reaction monitoring mode was used for quantitative analysis. An in-house library was constructed for identification. Calibration curves showed good linearity with correlation coefficients (r) higher than 0.994. Limits of detection were determined to be below 0.26 µg kg−1 for most analytes. The recoveries for those substances were in the acceptable range of 80.2%–119.1%. A new LC–MS3 method was established for further confirmation. One pickled pepper peanut was found to contain aflatoxins B1, B2, and G1 with contents of 90.93, 26.64, and 1.92 µg kg−1, respectively.
研究领域:
食品安全
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Current Pharmaceutical Analysis
·
2023
·Vol. 19
·期 4
·282-288
·
IF 0.6
Zhang Hanzhi,Qin Feng,Sun Ning,Zheng Mengmeng,Luo Wenyan,Qiu Ya,Liu Hao,Zhang Xiangmin
Background: After the hydrolysis of daptomycin in deuterated hydrochloric acid, the deuterium-substituted kynurenine was found, but the structure of deuterium-substituted kynurenine has not been reported. Introduction: The deuterium-substituted kynurenines were simply synthesized
and confirmed to be tri- and tetra-substituted products by high resolution mass spectrum and NMR. In further, the deuterium-substituted kynurenines were used to determine the conformation of kynurenine to be L-type in daptomycin through conformation analysis combined with derivation and high
performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLCQ/ TOF-MS). Methods: In the present study, a simple synthesis method was developed for deuteriumsubstituted kynurenine, and its structure was confirmed by high resolution mass spectrometry and NMR. L-kynurenine
was mixed with the deuterated hydrochloric acid and heated at 110 °C for 7 h. The hydrogen/deuterium exchange products of L-kynurenine were obtained through the hydrogen/deuterium exchange method. After the derivation of deuterium-substituted L-kynurenine by Marfey’s reagent, the
conformation of kynurenine in daptomycin was deduced by HPLC-Q/TOF-MS. Results: The deuterium-substituted kynurenines were confirmed to be tri- and tetra-substituted products by high resolution mass spectrum. Further, Hydrogen NMR spectrum indicated that the deuterium-substitution positions
were β-position on amino acid and 3’ and 5’ positions on the benzene ring. Thus, the tri-deuterium-substituted product was L-[β, 3’, 5’-2H3] kynurenine-d3, while the tetra-deuterium-substituted product was L-[β, β, 3’,
5’-2H4] kynurenine-d4. Furthermore, the deuterium-substituted kynurenines were used to determine the conformation of kynurenine to be L-type in daptomycin through conformation analysis combined with derivation and HPLC-Q/TOF-MS. Conclusion: The synthesis, structures,
and application of tri- or tetra- deuterium-substituted kynurenine were reported in this study.
研究领域:
生物化学
·
药物化学
·
分析化学
✓ 已验证
DOI
高影响因子
Analytical Methods
·
2015
·Vol. 8
·期 3
·666-672
·
IF 1.821
L. Chen,Y. Qin,X. Yang,C. Liu
An analytical method for the simultaneous determination of seven insecticides, including six neonicotinoids and one pyridine-azomethine, in drinks by LC-MS/MS using the Product Ion Confirmation Scan (PICS) mode was developed and validated. The compounds were extracted by modified QuEChERS and purified by d-SPE. The separation of all compounds was achieved in less than 3 minutes using a BEH C18 reverse-phase column and a mobile phase composed of 0.01% formic acid in water and methanol in the gradient elution mode at 0.4 mL min−1. Except for the two transitions and retention time demanded by EU/2002, identification was further carried out by matching the mass spectrum between the reference and sample produced by PICS if necessary. The LODs and LOQs for all compounds were lower than 0.014 μg L−1 and 0.05 μg L−1, respectively. The calibration curves were ranging from the LOQ to 0.02 mg L−1 with r2 higher than 0.9917 and reasonable recoveries were between 81.19% and 105.79% with RSD <15.0%. This work illustrates the advantages of using the PICS mode to build MRM acquisition methods in the application field of pesticide multi-residue analysis. It is very effective when only one MRM transition is obtained or the confirmation ion transition is too weak. It is proved that this is a rapid and reliable analytical method.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
Chinese Journal of Chromatography
·
2022
·Vol. 40
·期 5
·433-442
·
IF 0
Yangjie LI,Jiaying HUANG,Jihui FANG,Zhiye HUANG
A high throughput screening method based on ultra performance liquid chromatography-quadrupole-time-of-flight high resolution mass spectrometry (UPLC-Q-TOF HRMS) was developed for the simultaneous and rapid confirmation of 73 prohibited compounds in cosmetics. The sample was dispersed in a saturated sodium chloride solution and ultrasonically extracted using acetonitrile containing 0.2% (v/v) formic acid. The resultant solution was centrifuged and then cleaned using dispersive solid phase extraction using a primary secondary amine (PSA) sorbent. The purified solution was centrifuged, and the supernatant was filtered through a 0.22 μm membrane before determination. The optimal pretreatment method was determined by comparing the recovery rates obtained using different extraction solvents and different amounts of purifying agents. The chromatographic separation conditions and mass spectrometry scanning mode were also optimized. Chromatographic separation was performed on an Acquity UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) with gradient elution using 0.1% (v/v) formic acid aqueous solution and methanol as mobile phases. The eluent from the column was further detected using Q-TOF HRMS with the high resolution multiple reaction monitoring (MRM HR) scanning mode. Retention time, precise mass of parent ion, isotope abundance ratio, and precise mass of fragment ions were the parameters considered for rapid untargeted screening and confirmation. The matrix effects of water- and cream-based cosmetics were investigated. The matrix effects could be addressed using the matrix matched standard curve method. The correlation coefficients for the 73 prohibited compounds were all >0.99 in the corresponding linear concentration range. The limits of detection (LODs) were in the range of 5-150 μg/kg, and the limits of quantification (LOQs) were in the range of 15-450 μg/kg. Average recoveries were in the range of 60.3%-130.3% at three spiked levels, and the intra-day and inter-day precisions were 0.8%-10.0% ( n =6) and 1.1%-15.0% ( n =3), respectively. A total of 692 cosmetics samples were screened; 16 positive samples were detected, namely, sulfamethoxazole, meprednisone, lincomycin, 4-acetamidophenol, trimethoprim, alfacalcidol, betamethasone 17-valerate, brimonidine, chloramphenicol, chlorpheniramine, clobetasol propionate, crotamiton, econazole, ketoconazole, prednisone 21-acetate, and prednisone, with content in the range of 0.5-1136.1 mg/kg. The optimized method is accurate, fast, and simple, and it is suitable for the routine detection and rapid screening of common prohibited compounds in cosmetics. In addition, a screening and confirmation library was established for the 650 prohibited compounds using SCIEX OS and Library View software, using information-dependent acquisition (IDA)-MS/MS mode for MS data acquisition. The database contains multiple types of information, including formulas, theoretical exact mass, retention time, precise mass of parent ion, isotope abundance ratio, and fragment ion distribution. The library can be used for the simultaneous and rapid confirmation of prohibited compounds in cosmetics.
研究领域:
分析化学
·
化妆品科学
·
药物分析
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
Foods
·
2022
·Vol. 11
·期 8
·1155
·
IF 5.561
Jie-Biao Guo,Jin-Sheng Cheng,Tai-Long Wei,Fan-Min Wu,Gui-Hong Tang,Qing-Hua He
An immuno-separated assay for ochratoxin A detection coupled with a nano-affinity cleaning up for LC-confirmation was developed. Firstly, ochratoxin A was modified to quantum dot beads for immuno-fluorescent reporters. Secondly, Fe3O4magnetic nanoparticles were conjugated with protein G for immuno-magnetic adsorbents. The immuno-separation of fluorescent reporters by magnetic adsorbents could be completed by ochratoxin A, so the fluorescent reporters released from the immune complex indicate a linear correlation with the concentration of ochratoxin A. Furthermore, the immuno-separated ochratoxin A can be eluted from magnetic adsorbent for LC-conformation. The optimized assay showed results as follows: the quantitative range of the immuno-separated assay was 0.03–100 ng mL−1of ochratoxin A. The recoveries for spiked samples ranged from 78.2% to 91.4%, with the relative standard deviation (RSD) being 11.9%~15.3%. Statistical analysis indicated no significant difference between the HPLC-FLD results based on commercial affinity column and by nano-affinity cleaning up.Keywords:immuno-separated assay;nano-affinity cleaning up;immuno-magnetic adsorbent;immuno-fluorescent reporters;LC-confirmation
研究领域:
分析化学
·
毒理学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）