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PubMed2001

Fourteen-gauge ultrasonographically guided large-core needle biopsy of breast masses.

OBJECTIVE: Large-core needle biopsy of the breast can be performed with stereotactic or ultrasonographic guidance. However, ultrasonographically guided large-core needle biopsy has notable advantages, including the absence of ionizing radiation, increased patient comfort, and greater cost-effectiveness. The purpose of this study was to evaluate the accuracy of ultrasonographically guided large-core needle biopsy for the diagnosis of breast cancer in palpable and nonpalpable breast masses. METHODS: The study was a retrospective review of consecutive ultrasonographically guided large-core needle biopsies for indeterminate breast masses. A total 424 ultrasonographically guided core biopsies were performed in 367 patients with 1 or more breast masses. Ultrasonographically guided core biopsy was performed with a 14-gauge spring-loaded needle and a freehand technique. Correlation of ultrasonographically guided core biopsy pathologic findings with subsequent surgical pathologic findings or long-term imaging follow-up was performed. RESULTS: Of 424 indeterminate breast lesions for which histopathologic findings were obtained by ultrasonographically guided core biopsy, 234 cancers were diagnosed. Twenty-eight additional lesions had either questionable but not definitively malignant pathologic features (n = 11) or radiologic-pathologic discordance (n = 17) and were surgically excised. Of these, 8 additional cancers were diagnosed. Patients or surgeons chose excision of 41 additional lesions that were benign on ultrasonographically guided core biopsy No cancer was found in these surgical specimens. One additional cancer was diagnosed at a 6-month imaging follow-up because of interval growth. On the basis of surgical and long-term imaging follow-up, the sensitivity of ultrasonographically guided core biopsy for the diagnosis of breast carcinoma was 99.2% (95% confidence interval, 95.6%-99.9%) in 173 palpable breast masses and 93.2% (95% confidence interval, 87.1%-97%) in 251 nonpalpable masses. In cancers diagnosed on the basis of immediate surgical excision as a result of ultrasonographically guided core biopsy that showed either questionable pathologic features or radiologic-pathologic discordance, the sensitivity of ultrasonographically guided core biopsy for the diagnosis of breast cancer was 99.2%. CONCLUSIONS: Ultrasonographically guided large-core needle biopsy is a sensitive percutaneous biopsy method for the diagnosis of breast cancer in palpable and nonpalpable breast masses.

Adolescent↗

PubMed1997

Stability enhancement for peptide analysis by electrospray using the triple quadrupole mass spectrometer.

Electrospray ionization sources, used with triple quadrupole mass spectrometers from PE/Sciex (API III+), Micromass (Quattro II), and Finnigan (TSQ 7000), were modified with a 35-gauge stainless steel needle. The dimensions of the needle were 63 microm i.d. by 145 microm o.d. with variable length, depending on the specific instrument. This modification led to enhanced signal stability, improved signal/noise ratios, and lowered sample consumption for a wide range of peptides. Stable baselines were observed with flow rates in the range of 50 nL/min to 5 microL/min. An alternative design, based on a metal wire housed within a fused silica capillary, led to the most stable signals of all during infusion, but caused excessive peak broadening with capillary chromatography. The Finnigan interface was further modified with an external postcolumn addition tee, used in conjunction with capillary liquid chromatography columns of 30 and 50 microm internal diameter. The best results with the modified Finnigan interface were acquired using the 50-microm column at a flow rate of 150 to 200 nL/min.

Factor VII↗

PubMed1997

Influence of changes in ionized calcium on cardiovascular reactivity during hemodialysis.

In order to prevent hypercalcemia due to the treatment of secondary hyperparathyroidism the use of low calcium dialysate is advocated. However, as calcium ions play a pivotal role in both myocardial and vascular smooth muscle contraction, lowering the dialysate calcium concentration might result in a further impairment of the cardiovascular response during dialysis. Therefore, arterial blood pressure, forearm vascular resistance (FVR) and venous tone (VT) (straing-gauge plethysmography) as well as cardiac dimensions and output (echocardiography) were measured in 10 hemodynamically stable dialysis patients (ejection fraction > 30%) during two standardized sessions of three-hour combined ultrafiltration-hemodialysis (UF + HD) at two different dialysate calcium concentrations: 1.25 and 1.75 mmol/l. High calcium UF + HD resulted in a significant increase in plasma ionized calcium (+0.19 +/- 0.11 mmol/l; p < 0.01) while ionized calcium remained unchanged during low calcium UF + HD (-0.02 +/- 0.07 mmol/l). As a result, systolic, diastolic and mean arterial blood pressure were respectively 14 +/- 10, 5 +/- 7 and 9 +/- 9 mmHg higher during high calcium UF + HD as compared to low calcium UF +/- HD (p < 0.05). There were no significant differences in FVR and VT between the two treatments. During both treatments FVR increased while VT decreased. In addition, there were no differences in calculated systemic vascular resistance. However, with comparable end-diastolic dimensions, stroke volume (-18 +/- 13 ml) and cardiac output (-1.3 +/- 1.5 l/min) decreased significantly (p < 0.05) only during low calcium UF + HD. We conclude that even in hemodynamically stable patients changes in plasma ionized calcium are an important determinant of the blood pressure response during dialysis therapy. Whereas peripheral vascular reactivity is unaffected by changes in ionized calcium, myocardial contractility is improved with higher dialysate calcium concentrations.

Adult↗

PubMed1999

Characteristics and clinical application of a treatment simulator with Ct-option.

BACKGROUND AND PURPOSE: The integration of a scanner for computed tomography (CT) and a treatment simulator (Sim-CT, Elekta Oncology Systems, Crawley, UK) has been studied in a clinical situation. Image quality, hounsfield units (HU) and linearity have been evaluated as well as the implications for treatment planning. The additional dose to the patient has also been highlighted. MATERIAL AND METHODS: Image data is acquired using an array of solid state X-ray detectors attached externally to the simulator's image intensifier. Three different fields of view (FOV: 25.0 cm, 35.0 cm and 50.0 cm) with 0.2 cm, 0.5 cm and 1.0 cm slice thickness can be selected and the system allows for an aperture diameter of 92.0 cm at standard isocentric height. The CT performance has been characterized with several criteria: spatial resolution, contrast sensitivity, geometric accuracy, reliability of hounsfield units and the radiation output level. The spatial resolution gauge of the nuclear associates quality phantom (NAQP) as well as modulation transfer functions (MTF) have been applied to evaluate the spatial resolution. Contrast sensitivity and HU measurements have been performed by means of the NAQP and a HU conversion phantom that allows inserts with different electron densities. The computed tomography dose index (CTDI) of the CT-option has been monitored with a pencil shaped ionization chamber. Treatment planning and dose calculations for heterogeneity correction based on the Sim-CT images generated from an anthropomorphic phantom as well as from ten patients have been compared with similar treatment plans based on identical, yet diagnostic CT (DCT) images. RESULTS: The last row of holes that are resolved in the spatial resolution gauge of the NAQP are either 0.150 cm or 0.175 cm depending on the FOV and the applied reconstruction filter. These are consistent with the MTF curves showing cut-off frequencies ranging from 5.3 lp/cm to 7.1 lp/cm. Linear regression analysis of HU versus electron densities revealed a correlation coefficient of 0.99. Contrast, pixel size and geometric accuracy are within specifications. Computed tomography dose index values of 0.204 Gy/As and 0.069 Gy/As have been observed with dose measurements in the center of a 16 cm diameter and 32 cm diameter phantom, respectively for large FOV. Small FOV yields CTDI values of 0.925 Gy/As and 0.358 Gy/As which is a factor ten higher than the results obtained from a DCT under similar acquisition conditions. The phantom studies showed excellent agreement between dose distributions generated with the Sim-CT and DCT HU. The deviations between the calculated settings of monitor units as well as the maximum dose in three dimensions were less than 1% for the treatment plans based on either of these HU both for pelvic as well as thoracic simulations. The patient studies confirmed these results. CONCLUSIONS: The CT-option can be considered as an added value to the simulation process and the images acquired on the Sim-CT system are adequate for dose calculation with tissue heterogeneity correction. The good image quality, however, is compromised by the relative high dose values to the patient. The considerable load to the conventional X-ray tube currently limits the Sim-CT to seven image acquisitions per patient and therefore the system is limited in its capability to perform full three-dimensional reconstruction.

Computer Simulation↗

PubMed2006

A2e mediated phototoxic effects of endoilluminators.

AIMS: To compare the theoretical retinal threshold time for endoilluminators and experimental phototoxic effect using A2e laden retinal pigment epithelial (RPE) cells. METHODS: The spectral irradiances of three types of 20 gauge and 25 gauge endoilluminators, currently commercially available from two manufacturers, were evaluated in conditions where the total beam spectral power was divided by the beam spot size at an estimated use distance of 5 mm from the retina. The retinal threshold time was calculated using the guidelines recommended by the International Commission on Non-Ionizing Radiation Protection. In vitro, A2e laden cells were evenly exposed to light for 30 minutes with a standard endoilluminator positioned 1 cm above the cells and the cell viability was assessed by WST-1 assay. RESULTS: The retinal threshold times were within 1 minute for all the endoilluminators tested. A significant decrease in the viability of A2e laden RPE cells was observed after they were exposed to light from two of the three 20 gauge endoilluminators. Cell viability was not affected by the exposure to 25 gauge endoilluminators under the same conditions. There was no correlation between the theoretical threshold times and experimental data. CONCLUSIONS: Light exposure during vitrectomy can induce photochemical damage to the retina. Although the A2e laden RPE model may not correctly mimic a clinical situation, this model may be useful to estimate the possible photochemical damage to RPE cells that could not be deduced by a theoretical retinal hazard model.

Cell Line↗

PubMed1999

Percutaneous ultrasound-guided chemical parathyroid ablation for treatment of primary hyperparathyroidism in dogs.

OBJECTIVE: To evaluate the efficacy, feasibility, and safety of ultrasound-guided chemical ablation of parathyroid masses in dogs with primary hyperparathyroidism. DESIGN: Prospective clinical trial. ANIMALS: 8 dogs. PROCEDURE: In all dogs, a solitary parathyroid mass was evident ultrasonographically. Dogs were anesthetized with propofol, and a 27-gauge needle was directed into the parathyroid mass under ultrasound guidance. Ethanol (96%) was injected into the mass until there was evidence of diffusion of fluid throughout the mass. Serum total calcium, ionized calcium, phosphorus, and parathyroid hormone (PTH) concentrations were monitored daily for 5 to 7 days after the ablation procedure and again 1, 3, and 6 months after the procedure. Dogs were also monitored for adverse effects. Follow-up ultrasonography was performed 5 days and 1 month after the ablation procedure. RESULTS: One injection was required in 7 dogs, and 2 injections were required in 1. Serum total and ionized calcium concentrations were within reference ranges within 24 hours after treatment in 7 dogs and within 5 days in 1 dog. Serum PTH concentration decreased and serum phosphorus concentration increased within 24 hours after treatment in all 8 dogs. Transient hypocalcemia developed in 4 dogs during the first 5 days after treatment, but only 1 dog required treatment for hypocalcemic tetany. Hypercalcemia recurred in 1 dog 1 month after the procedure and surgical removal of the parathyroid mass was required. Other adverse effects were not reported. CONCLUSIONS AND CLINICAL RELEVANCE: Ultrasound-guided chemical ablation of parathyroid masses is a safe and effective alternative to surgery for dogs with primary hyperparathyroidism.

Adenoma↗

PubMed1989

Circadian rhythms for calcium, inorganic phosphorus, and parathyroid hormone in primary hyperparathyroidism: functional and practical considerations.

We obtained serial serum and urine samples from 14 patients with primary hyperparathyroidism both before and 3 to 9 months after excision of their parathyroid adenomas to (1) determine whether the circadian rhythms for calcium, phosphorus, and parathyroid hormone (PTH) previously described in normal human beings are disturbed in this disorder; (2) gauge the effect of surgical treatment on the patterns observed before intervention; and (3) ascertain whether time(s) of blood sampling can be defined for optimal biochemical detection of the disease. Significant rhythms for serum phosphorus, ionized calcium, PTH, urine phosphorus, and urine calcium were observed in many but not all patients before and after surgery. Nonetheless, collective analysis revealed the following: (1) diurnal patterns for serum ionized calcium, phosphorus, urine calcium, and urine phosphorus in patients with primary hyperparathyroidism both before and after surgery, whereas a rhythm for serum PTH was uniquely observed after surgical treatment; and (2) no significant correlation between preoperative serum ionized calcium and PTH but restoration of the expected reciprocal relationship between these variables after surgery. Although variability in individual expression of the rhythm for PTH precludes precise definition of a sampling "window" when hormone levels are likely to be highest, collection of data at points throughout the day helped establish the diagnosis of primary hyperparathyroidism in several patients with borderline serum biochemistries.

Adenoma↗

PubMed1996

Accurate measurement of copper-67 in the presence of copper-64 contaminant using a dose calibrator.

UNLABELLED: The use of 67Cu-labeled antibodies for the treatment of cancer has advanced to the clinical trial phase. Quantitation of 67Cu radiopharmaceuticals is complicated by the presence of the radioimpurity of 64Cu in 67Cu supplies. Here we report a method to assay 67Cu and 64Cu in a mixed sample with a commonly available instrument, the ionization chamber dose calibrator. METHODS: The activities of 67Cu and 64Cu in a mixed sample can be calculated from a single-dose calibrator measurement. The calculation requires (1) instrument-specific response coefficients D67 and D64, generated by gauging the instrument for the efficiency of measurement of 67Cu and 64Cu, and (2) a value for the ratio of 67Cu to 64Cu in the sample, routinely provided by major suppliers of 67Cu. D67 and D64 were empirically determined by measuring samples containing known amounts of 67Cu and 64Cu. The samples were also assayed by gamma ray spectroscopy to verify the isotope ratios given by the suppliers. RESULTS: This method generated accurate response coefficients. At the recommended dose calibrator setting for the measurement of 67Cu, at which D67 = 1.0, the measurement for D67 with this method was 1.02 (+/- 0.04). Isotope ratios provided by the radionuclide suppliers were corroborated by gamma ray spectroscopy. CONCLUSION: A method is presented by which 67Cu and 64Cu in a mixed sample can be assayed using a dose calibrator. Although the derived numeric constants are only correct for a specific dose calibrator and setting, the method can be adapted for use with any dose calibrator.

Calibration↗

PubMed2000

Managing a sound portable gauge radiation safety program.

At some construction engineering companies, individuals with no background in radiation safety sometimes are assigned the not always welcome title of Radiation Safety Officer (RSO). With this new title comes the responsibility of ensuring that portable gauges are used safely at their facilities and in tile field. These newly appointed RSOs sometimes lack the knowledge and experience needed to manage a radiation safety program. This article was developed to provide the basic information needed to work confidently and safely around these instruments and to discuss licensing requirements and other information pertaining to the management of a portable gauge radiation safety program.

California↗

PubMed2001

Percutaneous ultrasonographically guided radiofrequency heat ablation for treatment of primary hyperparathyroidism in dogs.

OBJECTIVE: To evaluate the efficacy and safety of ultrasonographically guided radiofrequency heat ablation of parathyroid masses in dogs with primary hyperparathyroidism. DESIGN: Clinical trial. ANIMALS: 11 dogs. PROCEDURE: In all dogs, either 1 or 2 parathyroid masses were evident ultrasonographically. Dogs were anesthetized, and a 20-gauge over-the-needle catheter was directed into the parathyroid mass via ultrasonographic guidance. Radiofrequency heat was applied to the stylet of the catheter until there was sonographically apparent change to the entire parenchyma of the mass. Serum total and ionized calcium and parathyroid hormone concentrations were monitored daily for 5 days after the ablation procedure and again at 1, 2, and 3-month intervals, if possible. Dogs were monitored for adverse effects. RESULTS: One treatment was required in 6 dogs, 2 treatments were required in 2 dogs, and treatment was unsuccessful in 3 dogs. Serum total and ionized calcium concentrations were within reference ranges within 2 days of the last procedure in all 8 successfully treated dogs. Serum parathyroid hormone concentration was decreased 24 hours after treatment in all 8 dogs. Hypocalcemia developed in 5 of the 8 successfully treated dogs, all of which required treatment. One dog had a transient voice change. Other adverse effects were not reported. CONCLUSIONS AND CLINICAL RELEVANCE: Ultrasonographically guided radiofrequency heat ablation of parathyroid masses is a safe and effective alternative to surgery in dogs with primary hyperparathyroidism.

Adenoma↗

PubMed2006

Combining drop-to-drop solvent microextraction with gas chromatography/mass spectrometry using electronic ionization and self-ion/molecule reaction method to determine methoxyacetophenone isomers in one drop of water.

A novel analytical technique termed drop-to-drop solvent microextraction (DDSME) was developed to determine three methoxyacetophenone isomers in one drop of water, which were then detected by gas chromatography/mass spectrometry using electronic ionization mass spectrometry for quantification analysis and self-ion/molecule reaction/tandem mass spectrometry for isomer differentiation. The best optimum parameters for the DDSME technique were as follows: extraction time, 5 min; using toluene as the extraction solvent; volume of extraction solvent, 0.5 microL and no salt addition. The advantages of this method are rapidity, convenience, ease of operation, simplicity of the device, and extremely little solvent and sample consumption. The limit of detection (LOD) for this technique was 1 ng/mL. The relative standard deviation was less than 2.6% (n = 5). The linear range of the calibration curve of DDSME is from 0.01 to 5 microg/mL with correlation coefficient (r2) of >0.954. In the comparison of the LOD of DDSME with other sample pretreatment methods including liquid/liquid extraction (LLE), single-drop microextraction (SDME), solid-phase microextraction (SPME), and liquid-phase microextraction (LPME) using a dual gauge microsyringe with hollow fiber methods, this method shows much better in sensitivity than the LLE (25 ng/mL) and it is compatible with SDME (0.5 ng/mL), SPME (0.5 ng/mL), and LPME using a dual gauge microsyringe with a hollow fiber (1 ng/mL). However, DDSME was more convenient than the LPME using a dual gauge microsyringe with a hollow fiber method and much lower cost than the SPME technique.

Acetophenones↗

PubMed2002

Local hypoxia is produced at sites of intratumour injection.

Intratumour injection, commonly used for gene or drug delivery but also associated with needle biopsy or insertion of invasive measuring devices, may damage tumour microvessels. To examine this possibility, SCCVII tumours grown subcutaneously in C3H mice were injected with a 26 gauge needle containing 0.1 ml of the fluorescent dye Hoechst 33342 to label cells lining the track of the needle. Hoechst-labelled cells sorted from these tumours were more sensitive to killing by hypoxic cell cytotoxins (tirapazamine, RSU-1069) and less sensitive to damage by ionizing radiation. Hoechst-labelled cells also bound the hypoxia marker pimonidazole when given by i.p. injection. Intratumour injection transiently increased hypoxia from 18 to 70% in the tumour cells adjacent to the track of the needle. The half-time for return to pre-treatment oxygenation was about 30 min; oxygenation of tumour cells along the track had recovered by 20 h after intratumour injection. This effect could have significant implications for intratumour injection of drugs, cytokines or vectors that are affected by the oxygenation status of the tumour cells as well as potential effects on biodistribution via local microvasculature.

Animals↗

PubMed1987

Computed tomography guidance for skeletal biopsy.

Computed tomographic (CT) guided biopsy and abscess drainage of multiple organ systems have been well described. Reports of spinal and skeletal applications have been less common. This study describes the use of CT guidance in the biopsy of various skeletal lesions in 46 patients. Forty-one patients had skinny needle aspirations (18 or 22 gauge) and 23 patients had trephine core biopsies. Sites of the lesions included: thoracic spine-15 patients, lumbosacral spine-17 patients, bony pelvis-6 patients, rib-2 patients, and long bones-6 patients. Fast scanners capable of rapid image reconstruction have overcome many constraints. With CT guidance, the physician who performs the procedure receives virtually no ionizing radiation. The exact location of the needle tip is accurately visualized in relation to the lesion being biopsied and to the vital organs.

Biopsy, Needle↗

PubMed2006

Direct combination of immersed single-drop microextraction with atmospheric pressure matrix-assisted laser desorption/ionization tandem mass spectrometry for rapid analysis of a hydrophilic drug via hydrogen-bonding interaction and comparison with liquid-liquid extraction and liquid-phase microextraction using a dual gauge microsyringe with a hollow fiber.

This study presents the feasibility of direct coupling of the immersed single-drop microextraction (SDME) technique with atmospheric pressure matrix-assisted laser desorption/ionization mass spectrometry (AP-MALDI-MS) for the rapid analysis of a hydrophilic drug (dopamine) from aqueous solution and human urine in an ion trap tandem mass spectrometer through hydrogen-bonding interaction of dopamine with the extraction solvent (octanol). The optimum conditions for the SDME experiments coupled to AP-MALDI/MS were: stirring rate, 240 rpm; extraction time, 5 min; sample pH value, 8; and matrix concentration, 2000 ppm, using alpha-cyano-4-hydroxycinnamic acid (alpha-CHCA) as matrix. The limits of detection (LODs) for the SDME/AP-MALDI-MS experiments were 25 and 40 ppm in water and human urine, respectively. In a comparison of this method with the traditional liquid-liquid extraction (LLE), the SDME method shows better LODs than the LLE (40 ppm) and the same LODs (25 ppm) as the liquid-phase microextraction using a dual gauge microsyringe with a hollow fiber (LPME/DGM-HF). However, the SDME method is more convenient than the LPME/DGM-HF method.

Atmospheric Pressure↗

PubMed2005

A serum proteomic approach to gauging the state of remission in Wegener's granulomatosis.

OBJECTIVE: To identify serum ion patterns that distinguish remission from active disease in patients with Wegener's granulomatosis (WG). METHODS: Using sera collected in the WG Etanercept Trial, we selected samples from patients who either were undergoing a period of extended disease remission or had recent flares of active WG. Unfractionated samples were randomized into sets for training and testing, such that remission sera and active disease sera could be analyzed without batch bias. Molecular species within the sera were ionized by high-resolution, matrix-assisted laser desorption ionization time-of-flight mass spectrometry. We then used a bioinformatics pattern-recognition tool to identify optimal combinations of ions. During the training stage, the clinical data (remission versus active disease) were provided in association with the spectral data from each sample. In the testing stage, we performed blinded testing on a previously unexamined set of samples. RESULTS: The most robust model, trained on a total of 82 samples (42 remission, 40 active disease), included 7 key ions with mass:charge ratios of 803.239, 2,171.672, 2,790.574, 3,085.237, 5,051.726, 5,833.989, and 6,630.465. The combined relative amplitudes of these 7 ions identified 5 distinct clusters of either remission or active disease samples during the training stage. In the testing stage, this model segregated 72 samples into the same 5 clusters, including 1 large remission cluster (n = 28) and another large active disease cluster (n = 32). Three smaller clusters of active disease or remission samples were also identified, with remission clusters populated by 2 samples in one cluster and 8 in another, and an active disease cluster populated by 2 samples. The model categorized 35 of 37 remission samples correctly (sensitivity 95%, 95% confidence interval [95% CI] 82.1-99.4) and 32 of 35 active disease samples correctly (specificity 91%, 95% CI 78.1-98.1). CONCLUSION: This serum proteomic profiling approach appears to be useful in distinguishing between states of stable clinical remission and active disease. Further validation and refinement of this strategy may help clinicians apply immunosuppressive therapies more judiciously among their patients, thereby avoiding morbidity and mortality from excessive treatment. Identification of the most robust and clinically useful combinations of ions will permit the rational selection of molecules for sequencing and analysis.

Antirheumatic Agents↗

PubMed1995

Depth of ionization chamber in water.

The device developed by the authors and described here enables the user to measure the depth from the water surface to the point of measurement for a cylindrical ion chamber with a waterproof plastic cap in a water phantom, free of surface-tension error with a high precision. The device seeks vertical orientation and provides the convenience of hands-free operation. The measurement process is simple and quick with a precision of 0.1 mm. (The device is currently available as a 'water phantom depth gauge' from Nuclear Associates, Division of Victoreen Inc., Clare Place, NY, USA.)

Biophysical Phenomena↗

PubMed2003

Jet expansion module for liquid-sampled GC-discharge ionization detection of liquefied gases.

A rugged jet expansion module was designed, built, and utilized to sample liquefied gas for gas chromatography-discharge ionization detector (GC-DID) analysis. The module is inserted at an intermediate stage between a higher pressure sample cylinder and lower pressure gas injection manifold. The title jet module permits selection of liquid-phase or vapor-phase sampling by setting the valve-cylinder orientation up or down (relative to gravity). It consists of a four-way stainless steel cross, plus the following components connected to pipe thread ports: (1) mechanical pressure gauge, -15 to +30 psig; (2) threaded nut with 0.010-in. jet orifice (connect to sample cylinder valve); (3) bellows valve (connect to GC manifold); (4) bellows valve (connect to expansion cylinder). Making use of the jet module, measurement of air concentration in [15N]ammonia and sulfur hexafluoride (single-component) samples was found to be significantly lower in the liquid phase by GC-DID. This compact apparatus enables phase-selective sampling, reduces primary manifold contamination, and improves operator safety.

Journal Article↗

PubMed2003

Liquid chromatography/tandem mass spectrometry methods for quantitation of mevalonic acid in human plasma and urine: method validation, demonstration of using a surrogate analyte, and demonstration of unacceptable matrix effect in spite of use of a stable isotope analog internal standard.

Selective, accurate, and reproducible liquid chromatography/tandem mass spectrometry (LC/MS/MS) methods were developed and validated for the determination of mevalonic acid, an intermediate in the biosynthesis of cholesterol and therefore a useful biomarker in the development of cholesterol lowering drugs, in human plasma and urine. A hepta-deuterated analog of mevalonic acid was used as the internal standard. For both methods, calibration standards were prepared in water, instead of human plasma and urine, due to unacceptably high levels of endogenous mevalonic acid. The lower quality control (QC) samples were prepared in water while the higher QC samples were prepared in the biological matrices. For the isolation/purification of mevalonic acid from the plasma and urine matrices, the samples were first acidified to convert the acid analyte into its lactone form. For the plasma samples, the lactone analyte was retained on and then eluted off a polymeric solid-phase extraction (SPE) sorbent. For the urine method, the sample containing the lactone analyte was passed through a C-18 SPE column, which did not retain the analyte, with the subsequent analyte retention on and then elution off a polymeric SPE sorbent. Chromatographic separation was achieved isocratically on a polar-endcapped C-18 analytical column with a water/methanol mobile phase containing 0.5 mM formic acid. Detection was by negative-ion electrospray tandem mass spectrometry. The standard curve range was 0.500-20.0 ng/mL for the plasma method and 25.0-1,000 ng/mL for the urine method. Excellent accuracy and precision were obtained for both methods at all concentration levels tested. It was interesting to note that for certain batches of urine, when a larger sample volume was used for analysis, a high degree of matrix effect was observed which resulted not only in the attenuation of the absolute response, but also in a change of analyte/internal standard response ratio. This demonstrated that, under certain conditions, the use of a stable isotope analog internal standard does not, contrary to conventional thinking, guarantee the constancy of the analyte/internal response ratio, which is a prerequisite for a rugged bioanalytical method. On the other hand, under conditions where the sample matrix does not have such a deleterious effect, we have found that a stable isotope analog could serve as a surrogate (substitute) analyte. Thus, we have shown that using calibration standards prepared by spiking plasma with tri-deuterated or tetra-deuterated mevalonic acid, instead of mevalonic acid itself (the analyte), plasma QC samples that contain mevalonic acid can be successfully analyzed for the accurate and precise quantitation of mevalonic acid. The use of a surrogate analyte provides the opportunity to gauge the daily performance of the method for the low concentration levels prepared in the biological matrix, which otherwise is not achievable because of the endogenous concentrations of the analyte in the biological matrices.

Chromatography, Liquid↗