HPLC法测定冻干粉针中AOH的含量

目的 :建立一种高效液相色谱法测定冻干粉针中A0H含量。方法 :采用Diamonsil C18色谱柱色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈-水(45:55);流速:1.0 m L/min;检测波长为206 nm;柱温25℃;进样体积:20μL。结果 :AOH主峰与有关物质分离良好,HPLC测定的线性范围为0.2mg/m L-0.8mg/m L(r=0.9994),该方法仪器精密度、日内精密度、日间精密度以及重复性RSD均在2%以下。结论 :用高效液相色谱法对冻干粉针中AOH进行含量测定,方法简单,结果准确可靠。     

HPLC法测定一种吡唑并嘧啶类原料药WL的含量和有关物质

目的 建立高效液相色谱法,测定一种吡唑并嘧啶类原料药WL的含量和有关物质.方法 采用Diamonsil C18(250mm×4.6mm,5 μm)色谱柱,以乙腈-水(40∶60)为流动相,流速1.0mL/min,检测波长269nm,柱温为室温.结果 WL检测浓度在8～ 120 μg/mL范围内与峰面积积分值呈良好的线性关系(r=0.9999);平均含量为99.5％,有关物质与主峰之间的分离度良好.检测限和定量限分别为2.16ng和7.2ng.结论 本法快速、简便、准确,专属性好,灵敏度高,可用于原料药WL的质量控制.     

HPLC法测定异咯嗪类S10注射液的含量

目的：建立一种反相高效液相色谱法测定S10注射液含量的方法。方法：采用Agilent Zarbox C18色谱柱（250mm×4.6mm,5μm）,以乙腈-四氢呋喃（8：1）为流动相A,水为流动相B进行梯度洗脱（0-10min,10%A→55%A;10-25min,55%A;25-27min,55%A→60%A;27-37min,60%A;37-42min,60%A→98%A;42-55min,98%A）,检测波长269nm,流速1.2mL/min,柱温为室温。结果：S10浓度在10-80μg/mL范围内与峰面积呈良好的线性关系（r=0.9999）,检测限和定量限分别为4ng和16ng,平均回收率分别是102.2%,102.3%,103.8%。结论：该高效液相色谱法快速、灵敏、可靠,专属性好,可用于S10注射液的含量测定。     

HPLC法测定异黄酮类化合物BI的含量及有关物质

目的：建立测定异黄酮类化合物BI的含量及有关物质的高效液相色谱方法。方法：采用AgilentZorbaxescilpseXDBC18（250mm×4．6mm,5．0μm）色谱柱;以0．15％醋酸-甲醇（45：55）为流动相;流速：1．OmL／min;检测波长为260nm;柱温40℃;进样体积：10μL。结果：在上述色谱条件下,各杂质及各降解产物均可与BI主峰良好分离,HPLC测定的线性范围为0．08μg-0．80μg（r=0．9999）,方法的仪器精密度、日内精密度、日间精密度及重复性的RSD均小于2％。结论：采用HPLC测定中药BI的含量及有关物质,方法简便,结果准确可靠。     

HPLC法测定陆英花和果实中齐墩果酸和熊果酸的含量

建立高效液相色谱法同时分离和测定陆英花和果实中齐墩果酸和熊果酸的含量。选用Kromasil C18色谱柱,流动相为甲醇：水：磷酸（90：10：0．2）,检测波长210nm,流速0．8mL／min,柱温25℃。齐墩果酸进样量在n55—5．50μg,熊果酸进样量在1．02—10．20μg时呈现良好的线性关系,相关系数均为0．9999,齐墩果酸和熊果酸的平均回收率分别为99．3％（RSD为1．9％）和101．2％（RSD为2．3％）.本法具有准确、灵敏、数据可靠的优点,可用于陆英花和果实的齐墩果酸和熊果酸的分离与测定。     

HPLC法测定陆英花和果实中齐墩果酸和熊果酸的含量

建立高效液相色谱法同时分离和测定陆英花和果实中齐墩果酸和熊果酸的含量。选用Kromasil C18色谱柱,流动相为甲醇∶水∶磷酸(90∶10∶0.2),检测波长210nm,流速0.8mL/min,柱温25℃。齐墩果酸进样量在0.55～5.50μg,熊果酸进样量在1.02~10.20μg时呈现良好的线性关系,相关系数均为0.9999,齐墩果酸和熊果酸的平均回收率分别为99.3%(RSD为1.9%)和101.2%(RSD为2.3%)。本法具有准确、灵敏、数据可靠的优点,可用于陆英花和果实的齐墩果酸和熊果酸的分离与测定。     

RP-HPLC法测定麦冬中麦冬皂苷D’的含量

目的:建立RP-HPLC法测定麦冬中麦冬皂苷D’的含量,方法:采用Diamonsil TMC18色谱柱(200mm×4.6mm,5μm),柱温为33℃,流动相为水-乙腈(体积比52∶48),流速0.80mL獉min-1,检测波长208nm.结果:麦冬皂苷D’的质量浓度在0.018~0.180mg·mL-1与峰面积呈良好的线性关系(r=0.999 9),平均回收率为99.5%(RSD=0.96%,n=9),结论:本方法简便,准确,可用于麦冬药材的质量控制。     

注射用己酮可可碱中己酮可可碱含量及有关物质的高效液相色谱法测定

目的:建立注射用己酮可碱中己酮可可碱含量及有关物质的高效液相色谱测定法.方法:采用Hy-persil C18(150×4.6mm,5μm)化学键合柱,以甲醇-水-冰醋酸(35∶65∶1)为流动相,检测波长为274nm.结果:己酮可可碱的线性范围为40～800ng,r=0.9995,检出限为1.2ng,定量限为4.0ng.结论:该方法简便准确,可用于注射用己酮可可碱产品的质量控制和生产过程监测.     

HPLC法同时测定复方利血平片中硫酸双肼屈嗪等5种成分

目的:建立同时测定复方利血平片中硫酸双肼屈嗪、氢氯噻嗪、维生素B1、维生素B6和泛酸钙5个成分的高效液相色谱法.方法:采用Inertsil oDS-SP (4.6mmx250mm,5μm)色谱柱,以缓冲液(0.11％己烷磺酸钠,0.02％庚烷磺酸钠混合溶液,每1000mL加0.2mL三乙胺,用5％磷酸溶液调节pH值至3.5)-乙腈-甲醇(70∶10∶20)为流动相,检测波长为210nm.结果:硫酸双肼屈嗪、氢氮噻嗪、维生素B1、维生素B6、泛酸钙的浓度分别在8.4～ 126.Sμg/mL(r=0.9997)、6.3～94.3 μ g/mL(r=0.9997)、2.0～29.5μg/mL(r=0.9997)、2.0～～ 29.Sμg/mL(r=0.9996)、2.2～29.8μg/mL(r=0.9996)范围内线性良好.平均回收率为96.5％～99.0％,RSD为0.6％～1.3％(n=15).结论:该方法可用于复方利血平片中硫酸双肼屈嗪、氢氮噻嗪、维生素B1、维生素B6、泛酸钙的测定.     

高效液相色谱法测定油类样品中的胆固醇含量

建立并验证了用高效液相色谱法测定油类样品中胆固醇含量的检测方法;方法:样品经无水乙醇-氢氧化钾溶液皂化后,石油醚和无水乙醇溶液提取,甲醇溶解定量后,高效液相色谱法检测,以相对保留时间定性,色谱峰面积定量;结果:该方法平均回收率为81.04%,RSD为1.15%,检测限(S/N=3)为1.11mg.L-1;结论:实验表明该方法准确可靠,回收率良好,对于地沟油的鉴定具有一定的借鉴意义。     

Comparison between two different designs in the AC voltage measurement

In this paper, a comparison is done between two different techniques in measuring the AC voltage. The first technique is the single junction thermal voltage converters (SJTVC) which consist of one thermal element (TE) which its output e.m.f. in the range of 7-12 mV and the other is the new designed thermal voltage converters which consist of a number of TEs connected in parallel, series and series/parallel to increase their output e.m.f. (becomes in the range of 35-51 mV). The effect of increasing the output e.m.f. is studied in this paper through evaluating the uncertainty budget and proved that its increase has a great effect on the accuracy and the uncertainty of the AC voltage measurement.     

高效液相色谱法测定花生中的黄曲霉毒素

黄曲霉毒素(AFT)的急性毒性很强,是重要的致癌物质。本文用甲醇水溶液提取花生样品中的AFT,提取液经过过滤、稀释后,用免疫亲和柱净化,以甲醇洗脱,用高效液相色谱法直接测定。方法的回收率为87％～101％,RSD<4％。     

高效液相色谱法测定蜂胶中的黄酮成分

蜂胶是一种纯天然物质,具有生理和药理活性。本文提出一种分析蜂胶及其制品中总黄酮成分的高效液相色谱法(HPLC)。该法采用甲醇回流提取其有效成分,能同时分离测定9种黄酮成分。回收率96.7％,变质系数4.1％。     

Comparison of threshold galling results from two testing methods

In this investigation, threshold galling tests were performed on several types of stainless steel using area contact and line contact testing procedures. The area contact test method employed was the ASTM standard G98, button-on-block test. In this test method, the end of a cylindrical button is placed in contact with a flat block at a desired contact pressure. The button specimen is rotated through one revolution and both specimens are visually inspected for the presence of galling. The line contact test method used was the button-on-cylinder test where the end of a stationary button contacts a cylinder along its length. After a given load is applied, the cylinder is rotated for a fixed number of cycles and the wear surfaces are inspected for galling. A comparison of the threshold galling results from each of the test methods is discussed in this report. Various testing conditions that influence the onset of galling are discussed, including sliding distance, surface oxide layer thickness, and stress distribution as well as the impact of the interpretation of experimental data on reported galling threshold magnitudes.     

Comparison of cervical musculoskeletal kinematics in two different postures of primate during voluntary head tracking

We have examined the effect on neck-muscle activation of altering whole body posture. A Rhesus monkey (Macaca mulatto) was trained to produce sinusoidal (0.25 Hz) head tracking movements in the sagittal plane when seated with trunk and head vertical or while standing in the quadrupedal position. Video-fluoroscopic images of cervical vertebral motion, and electromyographic (EMG) responses were recorded simultaneously. Results demonstrated that vertebral motion varied with body posture, occurring synchronously between all joints in the upright position and primarily at skull-C_i when in the quadrupedal position. Muscle EMG activation was significantly greater (p<0.00l) in the quadrupedal position than when upright for all muscles except semispinalis cervicis. Peak activation of all the muscles occurred prior to peak head extension in the quadrupedal position, suggesting synchronous activity between muscles. Data suggest that, when upright, muscles were activated in functional groupings defined by their anatomical arrangement. In the quadrupedal position, gravity acting on the horizontally oriented head produced greater activation and a collective response of the muscles.     

Comparison of in vitro valve pressure drop results from different investigators

Steady-state pressure-drop vs flow-rate measurements on prosthetic valves have been shown to correlate well with mean cyclic pressure drops vs RMS flow rate during systolic ejection from pulsatile flow data. The use of steady-state data is therefore validated as a means of assessing performance characteristics. Pressure-drop results reported in the literature were compared for valves of the same size and manufacture. Significant differences were noted, which are attributed to: (a) different geometries in the region of the valves, (b) different approach flow conditions, (c) different placement of pressure measurement taps, and (d) different methods of pressure measurement. Differences in pressure drop were observed to vary by as much as a factor of five among different investigators. The exponent n in the relation delta p infinity Q" was also observed to vary, depending on the above factors. The reasons for and some quantitative calculations on the observed differences are presented here.     

Comparison of EBSD patterns simulated by two multislice methods

The extraction of crystallography information from electron backscatter diffraction (EBSD) patterns can be facilitated by diffraction simulations based on the dynamical electron diffraction theory. In this work, the EBSD patterns are successfully simulated by two multislice methods, that is, the real space (RS) method and the revised real space (RRS) method. The calculation results by the two multislice methods are compared and analyzed in detail with respect to different accelerating voltages, Debye–Waller factors and aperture radii. It is found that the RRS method provides a larger view field of the EBSD patterns than that by the RS method under the same calculation conditions. Moreover, the Kikuchi bands of the EBSD patterns obtained by the RRS method have a better match with the experimental patterns than those by the RS method. Especially, the lattice parameters obtained by the RRS method are more accurate than those by the RS method. These results demonstrate that the RRS method is more accurate for simulating the EBSD patterns than the RS method within the accepted computation time.     

腹腔镜下不同子宫肌瘤剔除方式妊娠结局的比较

目的:比较不同子宫肌瘤剔除方式对妊娠结局的影响。方法:217例患者中注射垂体后叶素组84例(A组),子宫动脉阻断组61例(B组),单纯腹腔镜下子宫肌瘤剔除患者126例(C组)。比较3组患者手术情况、术后并发症、治疗效果及妊娠结局。结果:B组手术时间高于A组、C组,其术中出血量低于其他2组;A组、B组术中出血量、术后肛门排气时间、住院时间均低于C组,差异均有统计学意义(P<0.05)。A组、B组术后并发症发生率分别为4.92%(3/61)、5.95%(5/84),组间比较差异无统计学意义(P>0.05),C组术后并发症发生率为9.52%(12/126),高于其他2组,差异有统计学意义(P<0.05)。B组肌瘤残留率、复发率低于A组、C组,A组肌瘤残留率、复发率低于C组,差异有统计学意义(P<0.05)。3组患者妊娠时间、妊娠结局比较,差异无统计学意义(P>0.05)。结论:与单纯腹腔镜、局部注射垂体后叶素后子宫肌瘤剔除相比,子宫动脉阻断后切除病灶虽然技术要求较高,但能够在保证治疗效果与妊娠结局的前提下,进一步减少手术创伤、缩短术后恢复时间、降低术后并发症发生风险。