ABSTRACT
ABSTRACT: Objective To study the qualitative analysis strategy for unknown synthetic cannabinoid in the suspicious herbal product when no reference substance is available. Methods The synthetic cannabinoid in herbal blend was extracted with methanol. The extract was concentrated by rotary evaporator and separated and purified by preparative liquid chromatography, to obtain high purity synthetic cannabinoid sample. Gas chromatography-mass spectrometry ï¼GC-MSï¼, ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry ï¼UPLC-QTOF-MSï¼ and nuclear magnetic resonance ï¼NMRï¼ were used to determine the structure of the prepared compound. Results High purity unknown sample ï¼10 mgï¼ was obtained by preparative liquid chromatography. The sample was analyzed by GC-MS, UPLC-TOF-MS and NMR, and through spectrum analysis, the unknown synthetic cannabinoid was determined as 5F-EDMB-PICA. Conclusion The method to extract unknown synthetic cannabinoid from low content herbal products by preparative liquid chromatography was established, and the structure of the unknown sample was identified by comprehensive use of GC-MS, UPLC-QTOF-MS and NMR. The information will assist forensic laboratories in identifying this substance or other compounds with similar structures in their casework.
Subject(s)
Cannabinoids , Chromatography, High Pressure Liquid , Chromatography, Liquid , Gas Chromatography-Mass Spectrometry , Mass SpectrometryABSTRACT
ABSTRACT: Objective To establish an ion chromatography method for the salt form determination of new psychoactive substances ï¼NPSï¼. Methods The method of conducting qualitative and quantitative analysis of six types of organic acid ions ï¼acetate ion, tartrate ion, maleate ion, oxalate ion, fumarate ion, citrate ionï¼ and five types of inorganic anions ï¼fluoride ion, chloride ion, nitrate ion, sulfate ion, phosphate ionï¼ in NPS sample by ion chromatography was developed. The salt forms of 222 seized NPS samples ï¼103 samples with synthetic cannabinoids, 81 samples with cathinones, 44 samples with phenylethylamines, 12 samples with tryptamines, 7 samples with phencyclidines, 6 samples with piperazines, 2 samples with aminoindenes, 26 samples with fentanyls and 43 samples with other types of NPSï¼ were analyzed by this method. Results Each anion had good linearity in the corresponding linear range, the correlation coefficients ï¼rï¼ were greater than 0.999, the limits of detection were 0.01-0.05 mg/L, and the limits of quantitative were 0.1-0.5 mg/L. Except that 5F-BEPIRAPIM was hydrochloride, the salt forms of the other 102 synthetic cannabinoids were all base. The salt form of 81 cathinone samples, 44 phenylethylamine samples, 7 phencyclidine samples and 2 aminoindene samples were all hydrochloride. The salt forms of tryptamine samples included base, hydrochloride, fumarate and oxalate. The salt forms of piperazine samples included base and hydrochloride. The salt forms of fentanyl samples and samples of other types included base, hydrochloride and citrate. Conclusion Ion chromatography is a simple, accurate and efficient method for determining the salt form of NPS samples, which makes the qualitative and quantitative conclusions of NPS more scientific and rigorous.
Subject(s)
Psychotropic Drugs/chemistry , Chromatography, Liquid , Gas Chromatography-Mass Spectrometry , IonsABSTRACT
ABSTRACT: Objective To establish an infrared spectroscopic method for the rapid qualitative and quantitative analysis of caffeine and sodium benzoate in Annaka samples. Methods Qualitative and quantitative modeling samples were prepared by mixing high-purity caffeine and sodium benzoate. The characteristic absorption peaks of caffeine and sodium benzoate in Annaka samples were determined by analyzing the infrared spectra of the mixed samples. The quantitative model of infrared spectra was established by partial least squares ï¼PLSï¼. Results By analyzing the infrared spectra of 17 mixed samples of caffeine and sodium benzoate ï¼the purity of caffeine ranges from 10% to 80%ï¼, the characteristic absorption peaks for caffeine were determined to be 1 698, 1 650, 1 237, 972, 743, and 609 cm-1. The characteristic absorption peaks for sodium benzoate were 1 596, 1 548, 1 406, 845, 708 and 679 cm-1. When the detection of all characteristic absorption peaks was the positive identification criteria, the positive detection rate of caffeine and sodium benzoate in 48 seized Annaka samples was 100%. The linear range of PLS quantitative model for caffeine was 10%-80%, the coefficient of determination ï¼ R2ï¼ was 99.9%, the root mean square error of cross validation ï¼RMSECVï¼ was 0.68%, and the root mean square error of prediction ï¼RMSEPï¼ was 0.91%; the linear range of PLS quantitative model for sodium benzoate was 20%-90%, the R2 was 99.9%, the RMSECV was 0.91% and the RMSEP was 1.11%. The results of paired sample t test showed that the differences between the results of high performance liquid chromatography method and infrared spectroscopy method had no statistical significance. The established infrared quantitative method was used to analyze 48 seized Annaka samples, the purity of caffeine was 27.6%-63.1%, and that of sodium benzoate was 36.9%-72.3%. Conclusion The rapid qualitative and quantitative analysis of caffeine and sodium benzoate in Annaka samples by infrared spectroscopy method could improve identification efficiency and reduce determination cost.
Subject(s)
Caffeine , Sodium Benzoate , Chromatography, High Pressure Liquid , Least-Squares Analysis , Spectroscopy, Near-InfraredABSTRACT
ABSTRACT: Objective To study the identification method for 4'-F-4-methylaminorex ï¼4'-F-4-MARï¼ in samples without reference substance. Methods Gas chromatography-mass spectrometry ï¼GC-MSï¼, ultra-high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry ï¼UPLC-QTOF-MSï¼, nuclear magnetic resonance ï¼NMRï¼ and Fourier transform infrared ï¼FTIRï¼ were comprehensively used for the structure identification of 4'-F-4-MAR in samples. Results Under the positive electrospray ionization ï¼ESI+ï¼ mode, quasi-molecular ion in the first order mass spectrometry of the unknown compound was 195.092 6 and its molecular formula was inferred to be C10H11FN2O. The fragment ions in the mass spectrometry of the unknown compound were compared with the related fragment ions of 4,4'-dimethylaminorex ï¼4,4'-DMARï¼ in literature. It was found that the main fragment ions of the unknown compound were all 4 bigger than the corresponding fragment ions of 4,4'-DMAR. Therefore, the unknown compound was inferred to be a 4,4'-DMAR analogue with a methyl substituted by a fluorine in the benzene ring. The equivalent protons at δ=7.30 and δ=7.06 in 1H-nuclear magnetic resonance ï¼1H-NMRï¼ spectra and the characteristic spin-spin coupling constants ï¼1JC-F=245.2 Hz, 2JC-F=21.3 Hz, 3JC-F=8.1 Hzï¼ for 13C-19F interactions in carbon spectra, further proved that the fluorine substituted methyl at the para-position of the benzene ring. Finally, the unknown compound was determined as 4'-F-4-MAR. Conclusion A method that comprehensively used the identification materials 4'-F-4-MAR in GC-MS, UPLC-QTOF-MS, NMR and FTIR is established and the fragmentation mechanism of fragmentation ions of 4'-F-4-MAR created under the two modes -- electron impact ï¼EIï¼ and electrospray ionization under collision induced dissociation ï¼ESI-CIDï¼ is deduced. The information will assist forensic science laboratories in identifying this compound or other substances with similar structure in their case work.
Subject(s)
Aminorex , Spectrometry, Mass, Electrospray Ionization , Chromatography, High Pressure Liquid , Gas Chromatography-Mass Spectrometry , Mass Spectrometry , NitroimidazolesABSTRACT
ABSTRACT: Objective To provide the reference for the identification of unknown fentanyl analogues by studying the characteristic ions and main fragmentation pathways of fentanyl analogues in the modes of collision induced dissociation ï¼CIDï¼ and electron ionization ï¼EIï¼. Methods Nine fentanyl analogues ï¼2, 2'-difluorofentanyl, acetyl fentanyl, fentanyl, butyl fentanyl, valeryl fentanyl, acryloyl fentanyl, furan fentanyl, 4-fluorine isobutyl fentanyl, carfentanylï¼ were selected and analyzed with ultra-high performance liquid chromatography-quadrupole time-of-flight-mass spectrometry ï¼UHPLC-QTOF-MSï¼ and gas chromatography-mass spectrometry ï¼GC-MSï¼. The mass spectrum obtained was analyzed. The CID and EI fragmentation routes of fentanyl analogues were speculated. Results The CID and EI fragmentation pathways were highly similar. In the CID mode, characteristic ions were formed by the carbon-nitrogen bond cleavage between the piperidine ring and the N-phenyl-amide moiety, within the piperidine ring, and between the phenethyl and piperidine ring. While in the EI mode, dissociation of the piperidine ring, as well as cleavage between the piperidine ring and the phenethyl were the main fragmentation pathways. Conclusion This study summarizes the main fragmentation pathways and characteristic ions of fentanyl analogues in the CID and EI modes, which is useful for forensic laboratories to identify and structural analyze fentanyl type new psychoactive substance in practical work.
Subject(s)
Chemistry Techniques, Analytical/methods , Chromatography, High Pressure Liquid , Fentanyl/analysis , Gas Chromatography-Mass Spectrometry , Mass Spectrometry , Fentanyl/analogs & derivatives , HumansABSTRACT
Objective: To investigate the outcomes of coarctation resection and aortoplasty with autologous pulmonary artery patch for treating coarctation of the aorta combined with hypoplastic aortic arch in infants. Methods: Clinical data of 21 infants with coarctation of the aorta and hypoplastic aortic arch, who underwent coarctation resection and aortoplasty with autologous pulmonary artery patch in Fuwai hospital from January 2009 to June 2016 were retrospectively analyzed. The age of the patients was 4 (2, 5) months,and the body weight of the patients was (5.3±1.6) kg. The patients were followed up to observe the surgery effect. Results: No perioperative death and serious complications occurred. When the patients were discharged,the systolic blood pressure of the right upper limb was lower than the preoperative systolic blood pressure ((85.7±5.9) mmHg(1 mmHg=0.133 kPa) vs. (100.7±16.6) mmHg, P<0.001),and the systolic blood pressure of the right lower limb was higher than the preoperative systolic blood pressure ((98.7±13.3) mmHg vs. (85.6±20.8) mmHg, P<0.001). The pressure gradient of aortic coarctation detected by echocardiography was lower than the preoperative pressure gradient ((13.1±3.8) mmHg vs. (46.2±17.1) mmHg, P<0.001). No restenosis was detected by echocardiography at discharge. Follow-up data were obtained in 19 patients, and the follow-up time was 18 (8, 45) months.The patients grew well, and no death occurred. Restenosis occurred in 3 cases, 1 patient underwent aortic balloon dilatation and the remaining 2 patients were under follow up observation. Computed tomography angiography showed that the morphology of aortic arch was normal without signs of aortic aneurysm. Conclusion: Coarctation resection with autologous pulmonary artery patch aortoplastystrategy is considered as a safe and effective surgical method for management of infant coarctation with hypoplastic aortic arch, and this surgery method is related with satisfactory early and mid-term outcomes in this patient cohort.
Subject(s)
Aorta, Thoracic , Aortic Coarctation , Pulmonary Artery , Aorta , Aortic Coarctation/surgery , Follow-Up Studies , Humans , Infant , Pulmonary Artery/transplantation , Retrospective StudiesABSTRACT
Objective: To analyze the pathogens of lower respiratory tract infection(LRTI) including bacterial, viral and mixed infection, and to establish a discriminant model based on clinical features in order to predict the pathogens. Methods: A total of 243 hospitalized patients with lower respiratory tract infections were enrolled in Fujian Provincial Hospital from April 2012 to September 2015. The clinical data and airway (sputum and/or bronchoalveolar lavage) samples were collected. Microbes were identified by traditional culture (for bacteria), loop-mediated isothermal amplification(LAMP) and gene sequencing (for bacteria and atypical pathogen), or Real-time quantitative polymerase chain reaction (Real-time PCR)for viruses. Finally, a discriminant model was established by using the discriminant analysis methods to help to predict bacterial, viral and mixed infections. Results: Pathogens were detected in 53.9% (131/243) of the 243 cases.Bacteria accounted for 23.5%(57/243, of which 17 cases with the virus, 1 case with Mycoplasma pneumoniae and virus), mainly Pseudomonas Aeruginosa and Klebsiella Pneumonia. Atypical pathogens for 4.9% (12/243, of which 3 cases with the virus, 1 case of bacteria and viruses), all were mycoplasma pneumonia. Viruses for 34.6% (84/243, of which 17 cases of bacteria, 3 cases with Mycoplasma pneumoniae, 1 case with Mycoplasma pneumoniae and bacteria) of the cases, mainly Influenza A virus and Human Cytomegalovirus, and other virus like adenovirus, human parainfluenza virus, respiratory syncytial virus, human metapneumovirus, human boca virus were also detected fewly. Seven parameters including mental status, using antibiotics prior to admission, complications, abnormal breath sounds, neutrophil alkaline phosphatase (NAP) score, pneumonia severity index (PSI) score and CRUB-65 score were enrolled after univariate analysis, and discriminant analysis was used to establish the discriminant model by applying the identified pathogens as the dependent variable. The total positive predictive value was 64.7%(77/119), with 66.7% for bacterial infection, 78.0% for viral infection and 33.3% for the mixed infection. Conclusions: The mostly detected pathogens were Pseudomonas aeruginosa, atypitcal pathogens, Klebsiella pneumoniae, influenza A virus and human cytomegalovirus in hospitalized patients with LRTI in this hospital. The discriminant diagnostic model established by clinical features may contribute to predict the pathogens of LRTI.
Subject(s)
Bacteria/isolation & purification , Bacterial Infections/diagnosis , Bacterial Infections/microbiology , Polymerase Chain Reaction/methods , Respiratory Tract Infections/etiology , Virus Diseases/diagnosis , Virus Diseases/virology , Viruses/isolation & purification , Bacteria/genetics , Bacterial Infections/epidemiology , Humans , Infant , Inpatients , Mycoplasma pneumoniae , Pneumonia, Mycoplasma , Respiratory Tract Infections/epidemiology , Virus Diseases/epidemiology , Viruses/geneticsABSTRACT
Objective: To compare the clinical outcome of patients with pulmonary valve stenosis underwent transthoracic and percutaneous balloon pulmonary valvuloplasty. Methods: Clinical data of 806 patients diagnosed as pulmonary valve stenosis underwent transthoracic(171 patients as group A)or percutaneous balloon pulmonary valvuloplasty (635 patients as Group B) in Fuwai Hospital from February 2006 to January 2016 were analyzed retrospectively. There were 72 males in group A (42.1%) and 344 males in group B (54.2%). The average age was (1.6±1.1) years in group A and (21.0±18.5) years in group B. The median weight was 7.65 (7.68) kg (M(Q(R))) in group A and 43.75 (47.38) kg in group B. There were 732 (90.9%) patients followed up from 3 months to 10 years, with an average interval of (6.3±3.6) years. Sixty cases were ligated patent ductus arteriosus simultaneously, and 20 cases got Blalock-Taussig shunt at the same time of valvuloplasty in group A. There were 47 cases of transcatheter closure of atrial septal defect and 6 cases of transcatheter closure of patent ductus arteriosus in group B. The t test, rank sum test and χ(2) test were used to compare data of two groups. Results: There were no hospital death or cardiac tamponade and other serious complications for all patients. The postoperative hospital stayin group A was significantly longer than that in group B (8(5) days vs. 2(2) days, Z=-9.404, P=0.000). In every further consultation, patients were reviewed with transthoracic echocardiography to assess transpulmonary gradient and pulmonary regurgitation. There were significant difference between group A and B of preoperative transpulmonary pressure gradient ((80.6±22.4) mmHg vs.(72.6±20.5) mmHg, t=1.611, P=0.032, 1 mmHg=0.133 kPa) and so as transpulmonary pressure gradient reduction value ((55.9±21.0) mmHg vs. (46.6±23.4) mmHg, t=-1.710, P=0.026). Patients in both groups had good cardiac function during follow-up interval. One patient needed surgical valvuloplasty 10 months after percutaneous balloon pulmonary valvuloplasty and 1 case occurred moderate to severe tricuspid regurgitation in group B. During follow-up period, there was no significant difference between group A and B of transpulmonary pressure gradient ((22.3±6.5) mmHg vs. (25.2±12.6) mmHg, t=1.320, P=0.072), the incidence of pulmonary valve regurgitation in patients of group A was significantly lower than patients of group B (56.1% vs.65.2%, χ(2)=4.755, P=0.029). Conclusions: The clinical outcome and complications are similar between patients underwent two different routes of balloon pulmonary valvuloplasty. Transthoracic balloon pulmonary valvuloplasty is more suitable for infant and underweight children patients with pulmonary valve stenosis. Percutaneous balloon pulmonary valvuloplasty is more suitable for the treatment of the elder children or adults.