反相高效液相色谱／质谱法同时测定鸡肉中5种喹诺酮药物残留

采用反相高效液相色谱／四级杆串联质谱（RP-HPLC／MS／MS）同时测定鸡肉中的5种喹诺酮药物（quinolones，QNs）。均质后的鸡肉样品采用磷酸盐缓冲溶液和乙腈的混和溶液提取。提取液经正己烷液-液分配（LLP）去除脂肪后，用C18固相萃取（SPE）柱净化，氨化甲醇洗脱，洗脱液用氮气吹干，流动相定容后，分析物采用LC／MS／MS电喷雾电离（ESI），正离子，多反应监测（MRM）模式检测，外标法定量。在添加浓度2．5～10μg/kg范围内，5种QNs的回收率在79．8％～95．1％之间；相对标准偏差（RSD）均小于11．7％。环丙沙星、丹诺沙星、恩诺沙星检出限（LOD）为0．5μg／kg，沙托沙星为1．0μg／kg，氟甲喹为0．1μg／kg。     

HPLC of phenylthiocarbamyol labelled uridine-diphosphate-hexosamine

Summary The biochemical functions of uridine-diphosphate-amino-sugar conjugates are largely unknown. As a first step to investigate their biological roles in glycolysis of higher organisms, bovine heart muscle, which metabolizes large quantities of glycogen, was assayed for uridine-diphosphate-hexosamine. A low molecular mass ultrafiltrate was prepared from the methanolsoluble fraction of a beef heart homogenate, and the fraction was further purified using anion-exchange and reverse-phase HPLC. Samples were analyzed by two HPLC methods; anion-exchange in borate buffer and reverse-phase ion-pair chromatography. One newly established technique employing phenylthiocarbamoyl labelled uridine-diphosphate-hexosamine also was used selectively to separate uridine-diphosphate-hexosamine from other uridine-diphosphate-sugars. Hydrolysate of purified sample was classified further according to molecular structure. As a result, phenylthiocarbamoyl labelled HPLC is suitable and easy for the detection of uridine-diphosphate-hexosamine and its derivatives.     

Gradient-enhanced FAWSETS perfusion measurements

This work describes the use of custom-built gradients to enhance skeletal muscle perfusion measurements acquired with a previously described arterial spin labeling technique known as FAWSETS (flow-driven arterial water stimulation with elimination of tissue signal). Custom-built gradients provide active control of the static magnetic field gradient on which FAWSETS relies for labeling. This allows selective, 180 degrees modulations of the phase of the perfusion component of the signal. Phase cycling can then be implemented to eliminate all extraneous components leaving a signal that exclusively reflects capillary-level perfusion. Gradient-enhancement substantially reduces acquisition time and eliminates the need to acquire an ischemic signal to quantify perfusion. This removes critical obstacles to application of FAWSETS in organs other than skeletal muscle and makes the measurements more desirable for clinical environments. The basic physical principles of gradient-enhancement are demonstrated in flow phantom experiments and in vivo utility is demonstrated in rat hind limb during stimulated exercise.     

Epoxy-based electroactive polymer gels

We describe a new type of electroactive polymer gel. In contrast to cross-linked polyacrylates, this system is based on triepoxides cross-linked with polyfunctional amines. The stoichiometry is selected to form a cross-linked gel with excess amino hydrogens. In acid solutions these become cationic and the ionic interactions cause the gel to swell. We describe the mechanical properties of the gels, their response to changes in pH and to electrical activation. The response time is in rough agreement with what would be expected for a diffusional process through a gel of this size (about 100 μm). Samples of smaller dimensions would be expected to respond more rapidly.     

Quenching of Myosin Intrinsic Fluorescence Unravels the Existence of a High Affinity Binding Site for Decavanadate

Decavanadate, one of the aggregated species of vanadate, is a potent inhibitor of several enzymes, including skeletal muscle myosin. However, its putative binding sites in myosin are largely unknown. Titration of the intrinsic fluorescence of myosin, purified from rabbit skeletal muscle, have been carried out in 0.3 M KCl, 5 mM CaCl₂ and 25 mM Tris-HCl (pH 7.0), with 0.1 mg/ml myosin. In the 0-200 M total vanadate concentration range, decavanadate produced approximately 25% quenching of the intrinsic fluorescence of myosin, with an apparent dissociation constant in the micromolar range. This effect was found to be specific of decavanadate, because titration with metavanadate up to 200 M did not produce a significant quenching of the intrinsic fluorescence of myosin. This quenching was accompanied by a parallel decrease of the accessibility of myosin tryptophans to the water-soluble collisional quencher KI, with an apparent dissociation constant also in the micromolar range. It is concluded that the binding of decavanadate to high-affinity sites in myosin produces local conformational change(s) near the tryptophans more accessible to water in the three-dimensional structure of this protein.     

Sliding mode control of a “Soft” 2-DOF Planar Pneumatic Manipulator

This paper presents a sliding mode controller for a “Soft” 2-DOF Planar Pneumatic Manipulator actuated by pleated pneumatic artificial muscle actuators. Since actuator dynamics is not negligible, an approximate model for pressure dynamics was taken into account, which made it necessary to perform full input-output feedback linearization in order to design a sliding mode controller. The design of the controller is presented in detail, and experimental results obtained by implementing the controller are discussed Published in Prikladnaya Mekhanika, Vol. 44, No. 10, pp. 135–144, October 2008.     

Qualitative and Quantitative Evaluation of Some Vocal Function Parameters Following Fitting of a Prosthesis

The insertion of a prosthesis and restoration with pectoralis major myocutaneous flaps for patients subjected to total pharyngolaryngectomy is a technique now universally accepted; however the literature on the subject is lacking. Our study considers 10 patients subjected to total pharyngolaryngecto-my and restoration with pectoralis major myocutaneous flaps who were fitted with vocal function prostheses and a control group of 50 subjects treated with a total laryngectomy without pectoralis major myocutaneous flaps and who were fitted with vocal function prostheses. Specific qualitative and quantitative parameters were compared. The quantitative measurement of the levels of voice intensity and the evaluation of the harmonics-to-noise ratio were not statistically significant (p > 0.05) between the two study groups at either high- or low-volume speech. On the contrary, statistically significant differences were found (p < 0.05) for the basic frequency of both the low and the high volume voice. For the qualitative analysis seven parameters were established for evaluation by trained and untrained listeners; on the basis of these parameters the control group had statistically better voices.     

Ionic Polymer‐Metal Composite Actuators Employing Radiation‐Grafted Fluoropolymers as Ion‐Exchange Membranes

Summary: To develop ionic polymer‐metal composites (IPMC) with improved performance, three new ion‐exchange membranes were prepared and employed in IPMC construction. The membranes were prepared by radiation‐grafting of polystyrene sulfonic acid onto three fluoropolymers; poly(vinylidenefluoride‐co‐hexafluoropropylene), poly(ethylene‐co‐tetrafluoroethylene), and poly(tetrafluoroethylene‐co‐hexafluoropropylene). The bending displacements of the IPMCs constructed with these membranes were at least several times larger than that of Nafion IPMC of similar thickness without straightening‐back. The larger displacement was considered to be due to the higher concentration of ionic groups and consequent larger ion‐exchange capacity.

Actuation of (a) Nafion IPMC and (b) IPMC prepared in this study.     

On the relationship between swelling of myofibrils and their suspension rheology

The swelling of myofibrils extracted from white bovine muscle was followed by measuring their suspension rheology. Swelling of the myofibril with increasing pH and ionic strength was accompanied by an increase in both the steady shear viscosity of the suspension and the dynamic viscoelastic properties. Swelling was continuously monitored by measuringG while the ionic strength of the suspension was being changed by dialysis. The relationship between the degree of swelling and the rheological parameters is complicated because myofibrils are rodshaped and swell radially and therefore swelling results in a change in shape. To allow for this an attempt was made to generalize the data by plotting viscosity andG againstcS/ø _m , wherec is the protein concentration in the suspension,S is the swollen volume of the myofibrils per weight of protein, and ø _m is the maximum packing fraction.The best fit to the data was represented by the equations _sp = 1.05 (cS/ _m – 0.84)^1.23 Pa · sG = 8.78 (cS/ _m – 0.67)^2.22 N m^–2. The scatter was greatest forG, possibly because at low degrees of shear the myofibrils were associated and this was confirmed by optical microscopy. Pronounced non-Newtonian behavior was observed and it was suggested that this was due to the disruption of aggregate structures, although at low concentration, orientation of the rods in the shear field may also be important.