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At least 649 records · Page 36Linked to original sources
PubMed1999

Confirmation of avermectin residues in food matrices with negative-ion atmospheric pressure chemical ionization liquid chromatography/mass spectrometry.

A multi-residue LC/MS method has been developed to confirm avermectin drug residues in several food matrices. Ivermectin (IVR), doramectin (DOR), eprinomectin (EPR) and moxidectin (MOX) are confirmed using atmospheric pressure chemical ionization (APCI) with negative ion detection and selected ion monitoring of three to four ions for each compound. The drug residues are extracted from tissue or milk using previously published procedures. IVR and DOR are confirmed at 20 ppb levels in fortified salmon muscle; IVR is also confirmed in tissue from salmon dosed with the drug. Residues of DOR, IVR, and EPR are confirmed in fortified milk at the 20 ppb level and in fortified beef liver at 40 ppb. Residues of MOX can also be confirmed in these matrices, but at slightly higher levels (40-80 ppb).

Animals↗
PubMed2003

Ionization enhancement in atmospheric pressure chemical ionization and suppression in electrospray ionization between target drugs and stable-isotope-labeled internal standards in quantitative liquid chromatography/tandem mass spectrometry.

The phenomena of ionization suppression in electrospray ionization (ESI) and enhancement in atmospheric pressure chemical ionization (APCI) were investigated in selected-ion monitoring and selected-reaction monitoring modes for nine drugs and their corresponding stable-isotope-labeled internal standards (IS). The results showed that all investigated target drugs and their co-eluting isotope-labeled IS suppress each other's ionization responses in ESI. The factors affecting the extent of suppression in ESI were investigated, including structures and concentrations of drugs, matrix effects, and flow rate. In contrast to the ESI results, APCI caused seven of the nine investigated target drugs and their co-eluting isotope-labeled IS to enhance each other's ionization responses. The mutual ionization suppression or enhancement between drugs and their isotope-labeled IS could possibly influence assay sensitivity, reproducibility, accuracy and linearity in quantitative liquid chromatography/mass spectrometry (LC/MS) and liquid chromatography/tandem mass spectrometry (LC/MS/MS). However, calibration curves were linear if an appropriate IS concentration was selected for a desired calibration range to keep the response factors constant.

Artifacts↗
PubMed1996

Analysis of triacylglycerols by silver-ion high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.

Triacylglycerols of the seed oils rich in alpha- and/or gamma-linolenic acid moieties were separated by silver-ion high-performance liquid chromatography (HPLC) followed by on-line atmospheric pressure chemical ionization-mass spectrometric (APCI-MS) detection. Mass spectra of most triacylglycerols exhibited abundant [M + H]+ and [M - RCO2]+ ions, which defined the molecular weight and the molecular association of fatty acyl residues of a triacylglycerol, respectively. Silver ions formed weaker complexes with triacylglycerols containing gamma-linolenic acid than with those containing alpha-linolenic acid, i.e., the elution order of molecules was XYT gamma > XYT alpha, XT gamma T gamma > XT gamma T alpha > XT alpha T alpha, and T gamma T gamma T gamma > T gamma T gamma T alpha > T gamma T alpha T alpha > T alpha T alpha T alpha, where T alpha = alpha-linolenic acid, T gamma = gamma-linolenic acid, and X, Y = fatty acids different from linolenic acid. Furthermore, silver-ion HPLC resulted in partial separation within equally unsaturated triacylglycerols according to differences in the combined number of acyl carbons. Regioisomeric forms of triacylglycerols were not determined from the seed oil samples, although differences were measured with reference compounds in the relative abundances of [M - RCO2]+ ions formed by a loss of a fatty acyl residue from the sn-2 position and the sn-1/3 positions. Silver-ion HPLC/APCI-MS provided valuable information for structure elucidation of seed oil triacylglycerols: 43 molecular species were identified from cloudberry seed oil, 39 from evening primrose oil, 79 from borage oil, 44 from alpine currant, and 56 from black currant seed oils. The quantitation requires to be studied further, especially in those cases where several molecular weight species of triacylglycerols eluted in a single chromatographic peak.

Chromatography, High Pressure Liquid↗
PubMed2005

Determination of talinolol in human plasma using automated on-line solid phase extraction combined with atmospheric pressure chemical ionization tandem mass spectrometry.

A specific LC-MS/MS assay was developed for the automated determination of talinolol in human plasma, using on-line solid phase extraction system (prospekt 2) combined with atmospheric pressure chemical ionization (APCI) tandem mass spectrometry. The method involved simple precipitation of plasma proteins with perchloric acid (contained propranolol) as the internal standard (IS) and injection of the supernatant onto a C8 End Capped (10 mmx2 mm) cartridge without any evaporation step. Using the back-flush mode, the analytes were transferred onto an analytical column (XTerra C18, 50 mmx4.6 mm) for chromatographic separation and mass spectrometry detection. One of the particularities of the assay is that the SPE cartridge is used as a column switching device and not as an SPE cartridge. Therefore, the same SPE cartridge could be used more than 28 times, significantly reducing the analysis cost. APCI ionization was selected to overcome any potential matrix suppression effects because the analyte and IS co-eluted. The mean precision and accuracy in the concentration range 2.5-200 ng/mL was found to be 103% and 7.4%, respectively. The data was assessed from QC samples during the validation phase of the assay. The lower limit of quantification was 2.5 ng/mL, using a 250 microL plasma aliquot. The LC-MS/MS method provided the requisite selectivity, sensitivity, robustness accuracy and precision to assess pharmacokinetics of the compound in several hundred human plasma samples.

Automation↗
PubMed1998

Development of a method for quantitation of retinol and retinyl palmitate in human serum using high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.

A method for the quantitative analysis of the vitamin A compounds all-trans-retinol and all-trans-retinyl palmitate was developed using high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (APCI-LC-MS). Unlike previous quantitative mass spectrometric methods for vitamin A, HPLC separations were carried out using a C30 reversed-phase column instead of GC separation. Because no sample hydrolysis or derivatization was necessary, retinyl palmitate was preserved for analysis instead of being hydrolyzed to retinol. Human serum was analyzed following simple hexane extraction without saponification or any additional purification. A comparison of APCI and electrospray ionization showed that only APCI produced a linear response over all four orders of magnitude of retinol and three orders of magnitude of retinyl palmitate concentrations. Selected ion monitoring of the fragment ion of m/z 269 was used for APCI quantitation of both retinol and retinyl palmitate, since it was the base peak and the only abundant ion in the mass spectra of both compounds and the internal standard, retinyl acetate. The ion of m/z 269 corresponded to loss of water, loss of palmitic acid, or elimination of acetic acid from the protonated molecules of retinol, retinyl palmitate and retinyl acetate, respectively. The limit of detection of APCI-LC-MS for all-trans-retinol and all-trans-retinyl palmitate was determined to be approximately 34 fmol/microliter and 36 fmol/microliter (0.670 pmol all-trans-retinol and 0.720 pmol all-trans-retinyl palmitate injected in 20 microliters on-column), respectively. The limit of quantitation was approximately 500 fmol/microliter and 250 fmol/microliter (10 pmol and 5 pmol injected in 20 microliters on-column) for retinol and retinyl palmitate, respectively.

Chromatography, High Pressure Liquid↗
PubMed2004

A general atmospheric pressure chemical vapor deposition synthesis and crystallographic study of transition-metal sulfide one-dimensional nanostructures.

A series of transition-metal sulfide one-dimensional (1D) nanostructures have been synthesized by means of a general atmospheric pressure, chemical vapor deposition (APCVD) strategy. Vapour-liquid-solid (VLS) and vapour-solid (VS) mechanisms, along with the results of SEM and TEM observations, were used to explain the formation of these nanostructures. The regularity of the growth in the direction of the hexagonal nanowire is explored; we find that it prefers to grow along (1 0 0), (1 1 0), or (0 0 x) directions owing to particular crystal structures. The adopted synthetic route was expected to provide abundant useful 1D building blocks for the research of mesoscopic physics and fabrication of nanoscale devices.

Journal Article↗
PubMed2006

Ion chromatography-atmospheric pressure chemical ionization mass spectrometry for the determination of trace chlorophenols in clam tissues.

A novel analytical method has been developed for the determination of 14 trace chlorophenols in clam tissues by ion chromatography (IC) coupled with atmospheric pressure chemical ionization mass spectrometry (APCI-MS) in the negative mode. The method comprised a fast ultrasound-assisted extraction using a mixture of methanol/water (4:1v/v) containing 5% triethylamine (TEA) as extraction solvent, solid-phase extraction with an Oasis HLB cartridge and gradient separation using KOH/acetonitrile at a flow rate of 1.0 mL/min on an IonPac AG11 guard column (50 mm x 4.0 mm I.D.) and an IonPac AS11 analytical column (250 mm x 4.0 mm I.D.). The molecular ions m/z [M-H](-) 127, 129; 161, 163; 195, 197 and 263, 265, 267 were selected for quantification in the selected ion monitoring (SIM) mode for monochlorophenols (MCPs), dichlorophenols (DCPs), trichlorophenols (TCPs) and pentachlorophenol (PCP), respectively. The average recoveries of the objective compounds spiked in clam tissues were between 80.2% and 98.2%. Within-day and day-to-day relative standard deviations were less than 12.6% and 13.2%, respectively. The optimum IC-APCI-MS conditions were successfully applied to the analyses of 14 trace chlorophenols in clam tissues.

Animals↗
PubMed2004

Abatement of sulfur hexafluoride emissions from the semiconductor manufacturing process by atmospheric-pressure plasmas.

Sulfur hexafluoride (SF6) is an important gas for plasma etching processes in the semiconductor industry. SF6 intensely absorbs infrared radiation and, consequently, aggravates global warming. This study investigates SF6 abatement by nonthermal plasma technologies under atmospheric pressure. Two kinds of nonthermal plasma processes--dielectric barrier discharge (DBD) and combined plasma catalysis (CPC)--were employed and evaluated. Experimental results indicated that as much as 91% of SF6 was removed with DBDs at 20 kV of applied voltage and 150 Hz of discharge frequency for the gas stream containing 300 ppm SF6, 12% oxygen (O2), and 40% argon (Ar), with nitrogen (N2) as the carrier gas. Four additives, including Ar, O2, ethylene (C2H4), and H2O(g), are effective in enhancing SF6 abatement in the range of conditions studied. DBD achieves a higher SF6 removal efficiency than does CPC at the same operation condition. But CPC achieves a higher electrical energy utilization compared with DBD. However, poisoning of catalysts by sulfur (S)-containing species needs further investigation. SF6 is mainly converted to SOF2, SO2F4, sulfur dioxide (SO2), oxygen difluoride (OF2), and fluoride (F2). They do not cause global warming and can be captured by either wet scrubbing or adsorption. This study indicates that DBD and CPC are feasible control technologies for reducing SF6 emissions.

Air Pollutants↗
PubMed2004

A high-performance liquid chromatographic-atmospheric pressure chemical ionization-tandem mass spectrometric method for determination of risperidone and 9-hydroxyrisperidone in human plasma.

Risperidone, a benzisoxazole derivative, is an antipsychotic agent used for the treatment of schizophrenia. We developed a liquid chromatographic-atmospheric pressure chemical ionization-tandem mass spectrometric (LC-APCI-MS-MS) method with improved sensitivity, selectivity, and dynamic range for determination of risperidone and 9-hydroxyrisperidone in human plasma. A structural analogue of risperidone, RO68808 (5 ng/mL), is added as the internal standard to 1 mL of human plasma. Plasma is made basic, extracted with pentane/methylene chloride (3:1), the organic phase evaporated to dryness, and the residue is reconstituted in water with 0.1% formic acid/acetonitrile (20:1). For LC-MS-MS analysis, a Metachem Inertsel HPLC column (2.1 x 150 mm, 5-microm particle size) is connected to a Finnigan TSQ7000 tandem MS via the Finnigan API interface. Both electrospray (ESI) and APCI produced predominantly MH(+) ions for the two analytes and the internal standard. Ions detected by selected reaction monitoring correspond to the following transitions: m/z 411 to 191 for risperidone, m/z 427 to 207 for 9-hydroxyrisperidone, and m/z 421 to 201 for the internal standard. APCI provided a larger dynamic range (0.1 to 25 ng/mL) and better precision and accuracy than ESI. Intrarun accuracy and precision determined at 0.1, 0.25, 2.5, and 15 ng/mL were within 12% of target with %CVs not exceeding 10.9%. Interrun accuracy and precision determined at the same concentrations were within 9.6% of target with %CVs not exceeding 6.7%. Analytes were stable in plasma after 24 h at room temperature, 2 freeze-thaw cycles, and 490 days at -20 degrees C.

Antipsychotic Agents↗
PubMed2003

Application of 4-(4-nitrophenyl)-1,2,4-triazoline-3,5-dione to analysis of 25-hydroxyvitamin D3 in human plasma by liquid chromatography/electron capture atmospheric pressure chemical ionization-mass spectrometry.

The utility of 4-(4-nitrophenyl)-1,2,4-triazoline-3,5-dione (NPTAD) as a derivatization reagent in the analysis of 25-hydroxyvitamin D3 [25(OH)D3] using liquid chromatography/electron capture atmospheric pressure chemical ionization-mass spectrometry (LC/ECAPCI-MS) was examined. The derivatives of 25(OH)D3 with NPTAD underwent electron capture in the APCI source in the negative-ion mode and provided 30-fold higher sensitivity compared to an intact compound. This derivatization-LC/ECAPCI-MS method was applied to a plasma 25-hydroxyvitamin D3 assay, and gave satisfactory results in sensitivity, specificity, measurable range and throughput of the analysis.

Calcifediol↗
PubMed1991

Determination of small drug molecules by capillary electrophoresis-atmospheric pressure ionization mass spectrometry.

Capillary electrophoresis (CE) separations are reported for sulfonamides and benzodiazepines in an uncoated fused-silica capillary. The capillary column exit was connected to a liquid junction-ion spray interface combination coupled to an atmospheric pressure ionization (API) triple quadrupole mass spectrometric (MS) system. On-line UV detection occurred 20 cm from the inlet of the capillary and with the API mass spectrometer (CE-API-MS) after the entire length of the capillary (100 cm). The separations were made using volatile buffers composed of ammonium acetate (15-20 mM) with 15-20% of methanol to facilitate ionization under electrospray conditions. This study showed that the major metabolite of flurazepam in man, N-1-hydroxyethylflurazepam, could be detected and characterized in human urine by CE-UV-MS following the administration of a single oral dose of 30 mg of flurazepam dihydrochloride. The presence of additional flurazepam metabolites in human urine was observed by using the system, suggesting that a combination of UV with MS detection should be useful for metabolic studies. In addition to molecular weight determination of compounds, structural information may be obtained by utilizing online tandem mass spectrometry (CE-UV-MS-MS). This was demonstrated for sulfamethazine where the protonated molecule species was transmitted into the collision cell of the tandem triple quadrupole mass spectrometer. Collision-induced dissociation of the protonated sulfamethazine molecule yielded structural information characteristic of the sulfa drug following the on-column injection of 2 pmol of sulfamethazine.

Benzodiazepines↗
PubMed2005

Evaluation of diphenylamine derivatives in apple peel using gradient reversed-phase liquid chromatography with ultraviolet-visible absorption and atmospheric pressure chemical ionization mass selective detection.

A method was developed for extracting, identifying, and quantifying diphenylamine (DPA) derivatives in the peel of DPA-treated apples using gradient reversed-phase liquid chromatography with ultraviolet-visible absorption and atmospheric pressure chemical ionization detection (LC-UV-vis-APCI-MS). Compounds routinely analyzed using this method included hydroxylated, nitrosated, nitrated, and methoxylated diphenylamine derivatives. Analysis of peel treated with 0-8 g L(-1) DPA showed that peel DPA content was a limiting factor in derivative production and that recovery of most compounds over this range was linear.

Antioxidants↗
PubMed2000

Determination of sulfonamides by packed column supercritical fluid chromatography with atmospheric pressure chemical ionisation mass spectrometric detection.

Sulfonamide antibiotics are widely used to prevent bacterial infections in livestock, and residues are commonly found in milk and meat. Packed column supercritical fluid chromatography (pSFC) with detection using ultra violet (UV) and atmospheric pressure chemical ionisation (APCI) mass spectrometry (MS) provides a versatile method for the detection and quantification of six major sulfonamides. The APCI mass spectra for all the sulfonamides consisted of protonated molecules at low cone voltages. Increasing the cone voltage led to informative fragmentation patterns, which provided structural information for identification purposes. The pSFC-APCI-MS technique was shown to be linear (r2 > or = 0.999) over the concentration range 0.1-50 micrograms ml-1 using total ion current. The precision and the accuracy of the system and validation of sample preparation are acceptable, with RSD < 2% and relative error 8%. Selected ion monitoring gave detection limits as follows: sulfadiazine 41, sulfamethoxazole 45, sulfamerazine 47, sulfamethizole 59, sulfamethazine 181 and sulfadimethoxine 96 micrograms l-1, which are lower than the amounts permitted in milk products. The APCI pSFC-MS system was shown to have a high degree of reproducibility. The technique was then applied to determine the above sulfonamides in milk. The results obtained show that there are no matrix effects from the milk and that the detection limits remained as stated for the standard solutions.

Animals↗
PubMed2006

Analysis of 13 fentanils, including sufentanil and carfentanil, in human urine by liquid chromatography-atmospheric-pressure ionization-tandem mass spectrometry.

A sensitive, semiautomated method for the analysis of several fentanils and fentanil metabolites in human urine is described. This method uses solid-phase extraction of urine samples followed by liquid chromatography-atmospheric pressure ionization-tandem mass spectrometry. Isotopically labeled internal standards were included for 6 of the 13 analytes in this study. Estimated detection limits ranged from 3 to 27 pg/mL, and good accuracy and long-term precision were observed in most cases. This method should be useful for the rapid and sensitive screening of human urine samples for a number of fentanils and their metabolites as indicators of exposure.

Analgesics, Opioid↗
PubMed2004

Measurements of the indium hyperfine structure in an atmospheric-pressure flame by use of diode-laser-induced fluorescence.

We report on what we believe is the first demonstration of laser-induced fluorescence (LIF) in flames by use of diode lasers. Indium atoms seeded into an atmospheric-pressure flame at trace concentrations are excited by a blue GaN laser operating near 410 nm. The laser is mounted in an external-cavity configuration, and the hyperfine spectrum of the 5(2)P1/2 --> 6(2)S1/2 transition is captured at high resolution in single-wavelength sweeps lasting less than one tenth of a second. The research demonstrates the potential of diode-based LIF for practical diagnostics of high-temperature reactive flows.

Journal Article↗