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1.
Scand J Gastroenterol ; 54(10): 1226-1232, 2019 Oct.
Article in English | MEDLINE | ID: mdl-31532265

ABSTRACT

Background and Aims: A retrospective non-interventional, multi-centre patient chart review study was conducted to investigate the association of faecal calprotectin (FC) 1 year (±2 months) after biological therapy initiation with composite event-free survival (CEFS) consisting of surgical procedures, corticosteroid initiation, treatment failure or dose increase in patients with Crohn's disease (CD). In addition, the correlations of FC and other tests of disease activity were assessed.Materials and methods: Data on Finnish CD patients initiating a biological therapy between 2010 and 2016, were collected. The association of FC and CEFS was analysed with Kaplan-Meier and Cox proportional hazard modelling. The correlations were tested with Pearson's test.Results: Biological therapy was initiated in 186 patients, of which 87 (46.8%) had FC results available at 1 year and 80 had follow-up exceeding 14 months. The characteristics of patients with and without FC results were similar. Patients with elevated FC (>250 µg/g) had a significantly increased risk of experiencing composite event (HR 3.4, 95% CI: 1.3-8.9; p = .013) when compared to patients with normal FC (FC ≤ 100). No such risk was observed in patients with intermediately increased FC level (100 µg/g < FC ≤ 250 µg/g) (HR 2.2 (95% CI: 0.8-6.2; p = .120). FC value had significant positive correlation with CRP, HBI and leukocyte values when measured at similar timepoints.Conclusions: Elevated level of FC approximately 1 year after the initiation of biological therapy was associated with an increased risk of either surgical procedures, corticosteroid initiation, treatment failure or dose increase (i.e. composite outcome) in patients with CD.


Subject(s)
Crohn Disease/drug therapy , Feces/chemistry , Leukocyte L1 Antigen Complex/metabolism , Adolescent , Adult , Aged , Aged, 80 and over , Biomarkers/metabolism , Crohn Disease/metabolism , Crohn Disease/surgery , Dose-Response Relationship, Drug , Drug Administration Schedule , Drug Monitoring , Female , Finland , Follow-Up Studies , Humans , Kaplan-Meier Estimate , Male , Middle Aged , Proportional Hazards Models , Retrospective Studies , Severity of Illness Index , Treatment Outcome , Young Adult
2.
Dis Colon Rectum ; 51(4): 421-5, 2008 Apr.
Article in English | MEDLINE | ID: mdl-18213488

ABSTRACT

PURPOSE: This study was designed to evaluate prospectively the results of the overlap technique in primary sphincter reconstruction after obstetric tear. METHODS: Obstetric tears in 44 women were operated on with primary overlap reconstruction. These women were investigated six to nine months after the operation. Results were compared with those of a historical control group of 52 women whose obstetric sphincter rupture had been treated with the end-to-end technique. RESULTS: The overlap group had significantly more incontinence symptoms after delivery and repair of the sphincter tear than before delivery (P < 0.0001); however, their incontinence symptoms were significantly fewer than those of the end-to-end group (P = 0.004). The prevalence of persistent rupture of the external anal sphincter was significantly lower in the overlap group (6/44, 13.6 percent) than in the end-to-end group (39/52, 75 percent; P < 0.0001). Internal anal sphincter rupture occurred in 5 patients (11.4 percent) in the overlap group and in 40 patients (76.9 percent) in the end-to-end group (P < 0.0001). CONCLUSIONS: The overlap technique should be adopted as the method of choice for primary sphincter repair after obstetric tear.


Subject(s)
Anal Canal/injuries , Delivery, Obstetric/adverse effects , Digestive System Surgical Procedures/methods , Suture Techniques , Wounds and Injuries/surgery , Adult , Anal Canal/diagnostic imaging , Anal Canal/physiopathology , Colonoscopy , Defecation , Endosonography , Female , Follow-Up Studies , Humans , Manometry , Pressure , Retrospective Studies , Rupture , Treatment Outcome , Wounds and Injuries/diagnosis , Wounds and Injuries/etiology
3.
J Chromatogr A ; 1161(1-2): 275-83, 2007 Aug 17.
Article in English | MEDLINE | ID: mdl-17574560

ABSTRACT

Methodology for personal occupational exposure assessment of airborne trialkyl and triaryl organophosphates originating from hydraulic fluids by active combined aerosol and vapor sampling at 1.5L/min is presented. Determination of the organophosphates was performed by gas chromatography-mass spectrometry. Combinations of adsorbents (Anasorb 747, Anasorb CSC, Chromosorb 106, XAD-2 and silica gel) with an upstream cassette with glass fiber or PTFE filters and different desorption/extraction solvents (CS(2), CS(2)-dimethylformamide (50:1, v/v), toluene, dichloromethane, methyl-t-butyl ether and methanol) have been evaluated for optimized combined vapor and aerosol air sampling of the organophosphates tri-isobutyl, tri-n-butyl, triphenyl, tri-o-cresyl, tri-m-cresyl and tri-p-cresyl phosphates. The combination of Chromosorb 106 and 37 mm filter cassette with glass fiber filter and dichloromethane as desorption/extraction solvent was the best combination for mixed phase air sampling of the organophosphates originating from hydraulic fluids. The triaryl phosphates were recovered solely from the filter, while the trialkyl phosphates were recovered from both the filter and the adsorbent. The total sampling efficiency on the combined sampler was in the range 92-101% for the studied organophosphates based on spiking experiments followed by pulling air through the sampler. Recoveries after 28 days storage were 98-102% and 99-101% when stored at 5 and -20 degrees C, respectively. The methodology was further evaluated in an exposure chamber with generated oil aerosol atmospheres with both synthetic and mineral base oils with added organophosphates in various concentrations, yielding total sampling efficiencies in close comparison to the spiking experiments. The applicability of the method was demonstrated by exposure measurements in a mechanical workshop where system suitability tests are performed on different aircraft components in a test bench, displaying tricresyl phosphate air concentrations of 0.024 and 0.28 mg/m(3), as well as during aircraft maintenance displaying tri-n-butyl phosphate air concentrations of 0.061 and 0.072 mg/m(3).


Subject(s)
Aerosols , Air Pollutants/analysis , Gas Chromatography-Mass Spectrometry/methods , Organophosphorus Compounds/analysis , Adsorption , Humans , Occupational Exposure , Reference Standards , Sensitivity and Specificity , Spectroscopy, Fourier Transform Infrared
4.
Occup Environ Med ; 63(7): 482-7, 2006 Jul.
Article in English | MEDLINE | ID: mdl-16551754

ABSTRACT

OBJECTIVE: To study possible cross shift effects of environmental tobacco smoke (ETS) on pulmonary function among bar and restaurant employees before and after the implementation of a smoking ban in Norway. METHODS: The study included 93 subjects employed in 13 different establishments in Oslo. They were examined at the beginning and end of a workshift both while ETS exposure was present and when smoking was banned. The mean exposure level of nicotine and total dust before the ban was 28 microg/m3 (range 3-65) and 275 microg/m3 (range 81-506), respectively. Following the smoking ban, the mean level of nicotine and total dust was 0.6 mug/m3 and 77 microg/m3, respectively. Assessment of lung function included dynamic lung volumes and flows. RESULTS: The cross shift reduction in forced vital capacity (FVC) among 69 subjects participating in both examinations changed from 81 ml (SD 136) during exposure to ETS to 52 ml (SD 156) (p = 0.24) following the smoking ban. The reduction in forced expired volume in one second (FEV1) during a workshift, was borderline significantly reduced when comparing the situation before and after the intervention, by 89 ml (SD = 132) compared to 46 ml (SD = 152) (p = 0.09), respectively. The reduction in forced mid-expiratory flow rate (FEF25-75%) changed significantly from 199 ml/s (SD = 372) to 64 ml/s (SD = 307) (p = 0.01). Among 26 non-smokers and 11 asthmatics, the reduction in FEV1 and FEF25-75% was significantly larger during ETS exposure compared to after the smoking ban. There was an association between the dust concentration and decrease in FEF25-75% before the ban among non-smokers (p = 0.048). CONCLUSIONS: This first study of cross shift changes before and after the implementation of a smoking ban in restaurants and bars shows a larger cross shift decrease in lung function before compared with after the implementation of the ban.


Subject(s)
Occupational Diseases/etiology , Occupational Exposure/adverse effects , Pulmonary Disease, Chronic Obstructive/etiology , Smoking/adverse effects , Tobacco Smoke Pollution/adverse effects , Adult , Female , Humans , Male , Middle Aged , Nicotine/analysis , Norway/epidemiology , Occupational Diseases/epidemiology , Occupational Diseases/physiopathology , Occupational Exposure/analysis , Pulmonary Disease, Chronic Obstructive/physiopathology , Respiratory Function Tests , Restaurants , Smoking/legislation & jurisprudence
5.
J Chromatogr A ; 983(1-2): 43-50, 2003 Jan 03.
Article in English | MEDLINE | ID: mdl-12568369

ABSTRACT

Fast and sensitive packed capillary column switching liquid chromatography methodology has been developed for the determination of the pesticide rotenone in river water. Sample volumes of up to 1 ml are loaded onto a 23 x 0.25 mm, 5 microm Kromasil C18 packed capillary precolumn using a noneluting solvent composition of water-acetonitrile (99:1, v/v) at flow-rates up to 100 microl/min prior to solute backflushing onto a 200 x 0.32 mm, 3.5 microm Kromasil C18 packed capillary analytical column using a mobile phase of water-acetonitrile (30:70, v/v) at a flow-rate of 5 microl/min. The method was evaluated using river water samples spiked with rotenone in the concentration range 0.5-50 ng/ml using UV detection. The within-assay precision was between 5.0 and 7.7% relative standard deviation (RSD, n = 6) and the between assay precision was between 7.5 and 8.9% RSD (n = 6). The method was linear within the investigated mass range displaying a calibration curve correlation factor of 0.997. The mass limit of detection was 10 pg corresponding to a concentration limit of detection of 10 pg/ml, using time-of-flight mass spectrometry.


Subject(s)
Chromatography, Liquid/methods , Mass Spectrometry/methods , Rotenone/analysis , Spectrophotometry, Ultraviolet/methods , Water Pollutants, Chemical/analysis , Reproducibility of Results , Sensitivity and Specificity
6.
Ultrasound Obstet Gynecol ; 20(5): 496-501, 2002 Nov.
Article in English | MEDLINE | ID: mdl-12423489

ABSTRACT

OBJECTIVES: To evaluate transvaginal sonography with power Doppler capacity in the diagnosis of acute appendicitis and in discriminating appendicitis from pelvic inflammatory disease. PATIENTS AND METHODS: We describe transvaginal sonographic findings of six women with acute appendicitis selected from 31 women seen in an emergency room setting for clinically suspected pelvic inflammatory disease. The study population underwent gray-scale transvaginal sonography, and specific sonographic landmark findings for acute appendicitis and pelvic inflammatory disease were used. Hyperemia of any infectious complex was identified by power Doppler. Laparoscopy was performed after transvaginal sonography and was used as the gold standard. RESULTS: Laparoscopy showed acute appendicitis in six (19%) of the 31 patients. A thick walled non-compressible gas-containing tubular structure with a diameter exceeding 6 mm was seen by transvaginal sonography in four of the six cases, consistent with uncomplicated appendicitis. A heterogeneous complex with surrounding hyperechogenic soft tissue was seen in two cases with gangrenous appendicitis. Power Doppler detected hyperemia in all six cases. Normal adnexal structures were imaged next to the inflamed appendix. The sonographic criteria consistent with acute appendicitis were clearly different from those of acute pelvic inflammatory disease. CONCLUSIONS: Transvaginal sonography provides an opportunity to distinguish between appendicitis and acute pelvic inflammatory disease. Prospective trials are needed in order to evaluate the impact of transvaginal sonography in the diagnosis of acute appendicitis.


Subject(s)
Appendicitis/diagnostic imaging , Pelvic Inflammatory Disease/diagnostic imaging , Acute Disease , Adult , Diagnosis, Differential , Emergencies , Female , Humans , Sensitivity and Specificity , Ultrasonography, Doppler/methods
7.
Article in English | MEDLINE | ID: mdl-11820298

ABSTRACT

A miniaturized temperature-programmed packed capillary liquid chromatographic method with on-column large volume injection and UV detection for the simultaneous determination of the three selective serotonin reuptake inhibitors citalopram, fluoxetine, paroxetine and their metabolites in plasma is presented. An established reversed-phase C8 solid-phase extraction method was employed, and the separation was carried out on a 3.5-microm Kromasil C18 0.32x300 mm column with temperature-programming from 35 (3 min) to 100 degrees C (10 min) at 1.3 degrees C/min. The mobile phase consisted of acetonitrile-45 mM ammonium formate (pH 4.00) (25:75, v/v). The non-eluting sample focusing solvent composition acetonitrile-45 mM ammonium formate (pH 4.00) (3:97, v/v) allowed injection of 10 microl or more of the plasma extracts. The method was validated for the concentration range 0.05-5.0 microM, and the calibration curves were linear with coefficients of correlation >0.993. The limits of quantification for the antidepressants and their metabolites ranged from 0.05 to 0.26 microM. The within and between assay precision of relative peak height were in the range 2-22 and 2-15% relative standard deviation, respectively. The within and between assay recoveries were in the 61-99 and 54-92% range for the antidepressants, respectively, and between 52-102 and 51-102% for the metabolites.


Subject(s)
Chromatography, Liquid/methods , Citalopram/blood , Fluoxetine/blood , Paroxetine/blood , Selective Serotonin Reuptake Inhibitors/blood , Humans , Reproducibility of Results , Sensitivity and Specificity , Spectrophotometry, Ultraviolet
8.
J Chromatogr A ; 918(1): 221-6, 2001 May 18.
Article in English | MEDLINE | ID: mdl-11403451

ABSTRACT

Inverse temperature programming in packed capillary liquid chromatography coupled to evaporative light-scattering detection has been used to resolve native polyethylene glycol (PEG) oligomers. The model compound, PEG 1000, was separated on a 300 mm x 0.32 mm I.D. capillary column packed with 3 microm Hypersil ODS particles with acetonitrile-water (30:70, v/v) as mobile phase. The retention of the PEG oligomers increased with increasing temperature, different from what is commonly observed in liquid chromatography. The retention times of the oligomers were approximately doubled for each 25 degrees C increment of the column temperature in the temperature range 30-80 degrees C. The oligomers were almost unretained and co-eluted at a column temperature of 30 degrees C. At 80 degrees C a baseline separation of more than 22 peaks was obtained, but the last eluting peaks were severely broadened and all oligomers did not elute. When a negatively sloped temperature ramp from 80 to 25 degrees C at -1.5 degrees C/min was applied, the peak shapes were improved, additional peaks were detected and the analysis time was reduced by 48%. In the temperature programming mode, the intra-day precision of the retention times ranged from 0.5 to 5.8% (n=5).


Subject(s)
Chromatography, Liquid/methods , Polyethylene Glycols/isolation & purification , Polymers/isolation & purification , Temperature
9.
Ultrasound Obstet Gynecol ; 17(3): 233-8, 2001 Mar.
Article in English | MEDLINE | ID: mdl-11309174

ABSTRACT

OBJECTIVES: To evaluate the usefulness of power Doppler transvaginal sonography (TVS) in the diagnosis of pelvic inflammatory disease (PID) and to assess the diagnostic reliability of specific sonographic findings. POPULATION: The study population consisted of 30 women admitted for suspected acute PID. The reference group consisted of 20 women with proven hydrosalpinx formation. METHODS: Both conventional TVS and power Doppler TVS were performed. All patients with suspected acute PID underwent laparoscopy in order to confirm the diagnosis. Sonographic criteria described earlier were used for the diagnosis of acute PID. Power Doppler was used to assess the vascularity of any adnexal mass. RESULTS: Laparoscopy confirmed the diagnosis of PID in 20 (67%) of the 30 women with clinically suspected acute PID. Specific TVS findings, including wall thickness > 5 mm, cog-wheel sign, incomplete septa, and the presence of cul-de-sac fluid, discriminated women with acute PID from the control women with hydrosalpinx formation. Power Doppler TVS revealed hyperemia in all women with acute PID, but in only two women with hydrosalpinx (P = 0.01). Pulsatility indices were significantly lower in the acute PID group than in the control group (pulsatility index 0.84 +/- 0.04 vs. 1.50 +/- 0.10; P < 0.01). CONCLUSION: Power Doppler TVS was 100% sensitive and 80% specific in the diagnosis of PID (overall accuracy 93%). Specific sonographic landmark findings and power Doppler findings augment the clinical diagnosis of PID and allow simple classification of the severity of the disease.


Subject(s)
Pelvic Inflammatory Disease/diagnostic imaging , Ultrasonography, Doppler , Ultrasonography, Prenatal , Adolescent , Adult , Female , Humans , Laparoscopy , Middle Aged , Pelvic Inflammatory Disease/physiopathology , Pulsatile Flow , Reproducibility of Results , Sensitivity and Specificity
11.
J Chromatogr A ; 892(1-2): 67-74, 2000 Sep 15.
Article in English | MEDLINE | ID: mdl-11045481

ABSTRACT

A temperature-programmed packed capillary LC method with large-volume injection on-column focusing has been developed for screening and determination of 1-(2-methoxyphenyl)piperazine derivatives of airborne toluene-2,4-diisocyanate, toluene-2,6-diisocyanate, hexamethylenediisocyanate and methylenebisphenyl-4,4-diisocyanate, based on sampling methods described in MDHS 25/3. Injection volumes up to 100 microl were successfully loaded onto the 250x0.32 mm I.D. capillary column packed with 3 microm Hypersil ODS particles. The isocyanate derivatives were loaded at 10 degrees C and eluted by a three-step temperature program starting at 10 degrees C for 10 min, followed by a temperature ramp of 2.5 degrees C min(-1) to 45 degrees C and then 9.9 degrees C min(-1) to 90 degrees C. The mobile phase consisted of acetonitrile-acetate buffer (3% triethylamine, pH 4.5) (45:55, v/v). The isocyanate derivatives were dissolved in acetonitrile-acetate buffer (3% triethylamine, pH 4.5) (30:70, v/v) to achieve sufficient focusing. The concentration limit of detection of the individual derivatives utilizing an "U" shaped flow cell with a 8.0 mm light path and an injection volume of 100 microl was 44, 87, 43 and 210 pg ml(-1) for toluene-2,6-diisocyanate, hexamethylenediisocyanate, toluene-2,4-diisocyanate and methylenebisphenyl-4,4-diisocyanate, respectively. Within the investigated concentration range, 10-500 ng ml(-1), the linear calibration curves gave correlation coefficients ranging from 0.994 to 0.998. The repeatability of the method with regard to retention time and peak height ranged from 0.3 to 1.1% and 1.1 to 2.3% (n=9) relative standard deviation, respectively. The average recovery of the method, with regard to toluene-2,4-diisocyanate, was 97.7+/-1.6% (n=9).


Subject(s)
Chromatography, Liquid/methods , Isocyanates/chemistry , Piperazines/analysis , Reproducibility of Results , Sensitivity and Specificity , Temperature
12.
Hum Reprod ; 15(7): 1484-9, 2000 Jul.
Article in English | MEDLINE | ID: mdl-10875854

ABSTRACT

Chlamydia trachomatis infection is associated with pelvic inflammatory disease (PID) and tubal factor infertility (TFI). We investigated the role of C. trachomatis as a target antigen of endometrial and salpingeal tissue lymphocytes derived from PID and TFI patients. Antigen specificity of the tissue originated T lymphocyte lines (TLL) was tested against C. trachomatis elementary bodies and chlamydial heat shock protein 60 (CHSP60). C. trachomatis antigen stimulated proliferation in two out of eight endometrial TLL derived from PID patients and three out of four TLL derived from TFI patients. All (n = 4) TLL derived from the salpingeal specimens responded to CHSP60 compared with only one out of 12 TLL derived from the endometrial specimens. In-vivo expression of interferon-gamma (IFN-gamma) mRNA revealed that it was present in nine of 13 specimens obtained from PID patients. The dominant activity of type-1 T lymphocytes was confirmed by the in-vitro production of IFN-gamma (median 1007 pg/ml) from all (n = 5) C. trachomatis specific TLL while IL-5 secretion was lower (median 779 pg/ml). In conclusion, C. trachomatis reactive TLL were established from in-vivo activated lymphocytes from the upper genital tract tissue of PID and TFI patients. The reactivity of the salpingeal TLL to CHSP60 provided further evidence that immunoreactivity to CHSP60 is a predominant response in patients with tubal damage.


Subject(s)
Chlamydia trachomatis/immunology , Genitalia, Female/immunology , Infertility, Female/immunology , Pelvic Inflammatory Disease/immunology , T-Lymphocytes/immunology , Adolescent , Adult , Cell Division/drug effects , Cell Line/metabolism , Chaperonin 60/immunology , Chlamydia trachomatis/metabolism , Cytokines/metabolism , Female , Genitalia, Female/pathology , Humans , Infertility, Female/metabolism , Infertility, Female/pathology , Interleukins/pharmacology , Middle Aged , Pelvic Inflammatory Disease/metabolism , Pelvic Inflammatory Disease/pathology , T-Lymphocytes/pathology
13.
J Chromatogr Sci ; 38(4): 157-61, 2000 Apr.
Article in English | MEDLINE | ID: mdl-10766482

ABSTRACT

The effect of varying the operating temperature from 6 to 90 degrees C on the chromatographic performance of the exo-exo and exo-endo isomers of the X-ray contrast agent lodixanol in packed-capillary reversed-phase liquid chromatography shows increasing interconversion rates between the two isomeric conformers with increasing temperature. At 90 degrees C, Iodixanol elutes as one sharp peak due to an increased interconversion rate between the two isomeric conformers. Consequently, increased sensitivity is achieved. Temperature programming from 6 to 40 degrees C is utilized to optimize the resolution and determination of the exo-exo and exo-endo isomers. Temperature programming provides a significant decrease in the retention times in comparison with the isothermal separations while still preserving baseline separation of the isomers.


Subject(s)
Chromatography, Liquid/methods , Contrast Media/analysis , Triiodobenzoic Acids/analysis , Temperature
14.
J Am Assoc Gynecol Laparosc ; 7(1): 107-10, 2000 Feb.
Article in English | MEDLINE | ID: mdl-10648748

ABSTRACT

STUDY OBJECTIVE: To evaluate the efficacy of acute-phase operative laparoscopy in women with suspected pelvic inflammatory disease (PID). DESIGN: Open series (Canadian Task Force classification II-3). SETTING: University hospital. PATIENTS: Thirty-three patients with clinically suspected PID. INTERVENTION: Acute-phase operative laparoscopy. MEASUREMENTS AND MAIN RESULTS: Laparoscopy confirmed the diagnosis of PID in 20 (61%) patients; 11 (33%) women had other disease and 2 (6%) had no evidence of disease. Laparoscopic procedures in women with PID were pelvic irrigation (all patients), lysis of adhesions (most cases), drainage and irrigation of unilateral or bilateral pyosalpinx (7), drainage and irrigation of tubo-ovarian abscess (3), and extirpation of disease (2). Laparoscopic intervention was also performed in 11 (85%) of 13 women without PID. No major complications occurred. CONCLUSION: Acute-phase operative laparoscopy provided a final diagnosis in all but three patients (91%).


Subject(s)
Laparoscopy , Pelvic Inflammatory Disease/surgery , Acute Disease , Adult , Female , Humans , Pelvic Inflammatory Disease/diagnosis
16.
Radiology ; 210(1): 209-16, 1999 Jan.
Article in English | MEDLINE | ID: mdl-9885610

ABSTRACT

PURPOSE: To assess the value of magnetic resonance (MR) imaging in the diagnosis of pelvic inflammatory disease (PID) and to compare MR imaging with transvaginal ultrasonography (US) and laparoscopy. MATERIALS AND METHODS: Thirty consecutive patients hospitalized because they were clinically suspected of having PID underwent transvaginal US and T1-weighted spin-echo, T2-weighted turbo spin-echo, and inversion-recovery MR imaging at 1.5 T. All patients underwent laparoscopy after MR imaging. RESULTS: PID was laparoscopically proved in 21 (70%) patients. The MR imaging diagnosis agreed with that obtained with laparoscopy in 20 (95%) of the 21 patients with PID. The imaging findings for PID were as follows: fluid-filled tube, pyosalpinx, tubo-ovarian abscess, or polycystic-like ovaries and free pelvic fluid. Findings at transvaginal US agreed with those at laparoscopy in 17 (81%) of the 21 patients with PID. The sensitivity of MR imaging in the diagnosis of PID was 95%, the specificity was 89%, and the overall accuracy was 93%. For transvaginal US, the corresponding values were 81%, 78%, and 80%. CONCLUSION: MR imaging is more accurate than transvaginal US in the diagnosis of PID and provides information about the differential diagnosis of PID. MR imaging may reduce the need for diagnostic laparoscopy.


Subject(s)
Laparoscopy , Magnetic Resonance Imaging , Pelvic Inflammatory Disease/diagnosis , Adolescent , Adult , Diagnosis, Differential , Female , Humans , Middle Aged , Pelvic Inflammatory Disease/diagnostic imaging , Prospective Studies , Ultrasonography
17.
J Chromatogr A ; 864(1): 103-9, 1999 Dec 09.
Article in English | MEDLINE | ID: mdl-10630875

ABSTRACT

Sub-ambient column temperatures, promoting strong interactions between the analyte and the stationary phase material, were utilized to focus large volumes of the polyolefin antioxidant Irganox 1076 [benzenepropanoic acid, 3.5-bis(1,1-dimethylethyl)-4-hydroxy-, octadecyl ester] on the column inlet, using pure acetonitrile as sample solvent and mobile phase. Injection volumes up to 100 microl were successfully employed on a 50 cm x 320 microm I.D. capillary column packed with 5 microm Kromasil 100 ODS particles. Irganox 1076 was eluted after completed injection by temperature programming, using a temperature program from 7 to 90 degrees C, in 3 degrees C min(-1). UV detection, using a low-dispersion "U"-shaped flowcell, was performed at 280 nm. The method was applied for the determination of Irganox 1076 that was extracted from low-density polyethylene (0.6 ppm, w/w). Both Soxhlet and microwave-aided solvent extractions were performed, using chloroform and acetonitrile as solvents, respectively. The microwave-aided extraction with acetonitrile was found to give approximately the same yield as the standard Soxhlet reference method. Consequently, small volumes of acetonitrile could be used both as extraction solvent, sample solvent and mobile phase, simplifying the analysis process. The mass limit of detection of the method was found to be 3.3 ng, corresponding to a concentration limit of detection of 33 ng ml(-1), utilizing an injection volume of 100 microl. The within and between day precision of retention times displayed relative standard deviations below 1.2%.


Subject(s)
Antioxidants/analysis , Butylated Hydroxytoluene/analogs & derivatives , Chromatography, Liquid/methods , Acetonitriles , Butylated Hydroxytoluene/analysis , Chloroform , Polyethylene , Solutions , Solvents , Temperature
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