液相色谱-串联质谱技术在临床检验中的应用研究进展

液相色谱-串联质谱（LC-MS/MS）技术具有高灵敏度、高特异性、高分辨率和高效率的优点。近年来随着仪器灵敏度的提高，LC-MS/MS在常规临床检验中显示出极大的潜力，并在疾病早期预防和诊断中发挥着不可替代的作用。本文对LC-MS/MS在新生儿疾病筛查、维生素D检测、内分泌激素检测、肽类和蛋白质定量分析等临床检验方面的研究进展进行综述，并讨论了未来面临的挑战。     

Effect of wind condition on unintended hydrogen release in a hydrogen refueling station

Ambient condition, especially the wind condition, is an important factor to determine the behavior of hydrogen diffusion during hydrogen release. However, only few studies aim at the quantitative study of the hydrogen diffusion in a wind-exist condition. And very little researches aiming at the variable wind condition have been done. In this paper, the hydrogen diffusion in different wind condition which including the constant wind velocity and the variable wind velocity is investigated numerically. When considering the variable wind velocity, the UDF (user defined function) is compiled. Characteristics of the FGC (flammable gas cloud) and the HMF (hydrogen mass fraction) are analyzed in different wind condition and comparisons are made with the no-wind condition. Results indicate that the constant wind velocity and the variable wind velocity have totally different effect for the determination of hydrogen diffusion. Comparisons between the constant wind velocity and the variable wind velocity indicate that the variable wind velocity may cause a more dangerous situation since there has a larger FGC volume. More importantly, the wind condition has a non-negligible effect when considering the HMF along the radial direction. As the wind velocity increases, the distribution of the HMF along the radial direction is not Gaussian anymore when the distance between the release hole and the observation line exceeds to a critical value. This work can be a supplement of the research on the hydrogen release and diffusion and a valuable reference for the researchers.     

超高效液相色谱-串联质谱法同时检测糕点中6种甜味剂

目的建立超高效液相色谱-串联质谱法同时测定糕点中6种常用合成甜味剂的分析方法。方法选用超纯水作为提取溶剂,涡旋和超声提取后,低温离心,取部分上清液加入正己烷除脂,Waters Atlantis■T3色谱柱、甲醇-5 mmol/L甲酸铵(含0.1%甲酸)作为流动相、亲水亲脂平衡型固相萃取柱HLB(hydrophile-lipophile balance)净化。结果6种甜味剂在质量浓度为10~200 ng/mL的曲线范围内呈良好线性关系,相关系数r均大于0.999,平均加标回收率在85.0%-98.2%之间,相对平均偏差(relative standard deviation,RSD)为1.3%~6.7%。结论该方法具有前处理简单、灵敏度高、检测速度快等优点,适合糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、纽甜的检测,但不适用于安赛蜜的检测。     

Thermal prehistory,structure and high-temperature thermodynamic properties of Y2O3-CeO2 and Y2O3-ZrO2-CeO2 solid solutions

Ceria-based solid solutions are important materials for high- and medium-temperature electrochemical applications. However, the stabilities of both binary and ternary ceria-based solid solutions are insufficient at elevated temperatures, which limits their application as solid electrolytes or SOFC cathodes. Data on the high-temperature stability of ceria-based ceramics are unavailable in the literature. In the present study, we report a thermodynamic stability investigation of Y₂O₃-CeO₂ and Y₂O₃-ZrO₂-CeO₂ solid solutions. The thermal prehistories of binary and ternary systems were investigated using STA, XRD, and ESCA techniques. The vaporization processes were investigated in the temperature range of 1577–2227°С via the Knudsen effusion mass spectrometry technique. Using data on the component activity in solid-phase thermodynamic properties of Y₂O₃-CeO₂ solid solutions, which is represented as the Gibbs energy, the excess Gibbs energy was calculated as a function of the ceria mol. %. It was shown that the reduction of Ce⁴⁺ to Ce³⁺ in Y₂O₃-CeO₂ and Y₂O₃-ZrO₂-CeO₂ solid solutions corresponds to less-negative Gibbs energy compared to ZrO₂-CeO₂ solid solutions.     

Characteristic tryptic peptides and gelling properties of porcine skin gelatin affected by thermal action

Thermal action in extraction process had effects on characteristic tryptic peptides identification and gelling properties of porcine gelatin. SDS-PAGE, HPLC-LTQ/Orbitrap high-resolution mass spectrometry, texture analyser and rheometer were used to evaluate collagen depolymerisation degree, characteristic tryptic peptides and gelling properties of gelatins prepared in various thermal actions. Results showed that with increasing temperature and time, depolymerisation degree enlarged, while gel strength, gelling and melting temperature decreased. Mass spectra showed that 47 and 49 common characteristic tryptic peptides were identified in gelatins extracted at 50 °C and 100 °C with various times, respectively. Moreover, 34 common characteristic tryptic peptides were identified in all gelatin samples. Further comparison between this work and our previous investigations yielded 20 common characteristic tryptic peptides, which stably exist in various thermal actions. These common characteristic tryptic peptides may be very helpful for the accurate authentication of porcine gelatin.     

不同段数爆破地震波的反应谱分析

为了研究段数对反应谱特性的影响,基于某石方控制爆破工程爆破振动实测数据,对不同段数爆破振动信号进行了反应谱分析。首先,利用实测的爆破振动速度信号采用直接微分法获得了加速度信号,并利用EEMD分解对加速度信号进行低通滤波去噪处理,获得了准确清晰的加速度曲线。然后,利用精确法求得了不同段数下爆破振动信号的速度反应谱和标准速度反应谱。分析结果表明:不同段数的爆破振动质点峰值速度与速度反应谱的峰值速度并不存在对应关系,因此分段数的选择应综合考虑结构对爆破振动的动态响应。     

应用独立分量分析的激光测风雷达湍流频谱分解

针对大型风力发电机机组中常见的脉动湍流、风机尾流与涡流等湍流信号,研究了利用自然梯度下降的独立分量分析方法的湍流频谱分离效果,以区分中心风速与湍流信号,提高风机机组的综合工作效率。首先分析了风机组中常见湍流信号的后向散射与频谱分布特点,然后依据这些特点设计了对应的独立分量分析模型。在仿真结果符合要求的基础上,进行了双目激光雷达天线的风速采集与实际分离效果检测。实验结果表明,在大气折射率结构常数C2n≤10-14同时广义大气常数α≥4的通常情况下,利用双目信号能够分离出一个湍流中心和一个中心风速。对1 s内两个谱峰的波动范围进行统计,获得(2.59±0.05)MHz的中心风速以及(1.22±0.19)MHz的湍流中心估计,且二者的平均信噪比分别为25.93 dB和31.01 dB,能够在获得稳定的中心风速估计的同时得到一个较为稳定的湍流中心估计。     

不同工质回路热管负载功率变化下的质量流量特性

为了进一步提高回路热管仿真精度并丰富回路热管实验研究方法，本文对回路热管瞬态传质进行实验研究。使用高精度质量流量计分别对以丙酮、乙醇、丙烯为工质的回路热管进行不同负载功率下的质量流量测量研究。结果表明：启动阶段，热负载10W时，丙烯回路比丙酮回路热管启动快，且两者的温度稳定均滞后于质量流量；稳定阶段，随着热负载功率增大，不同工质的回路热管的平均质量流量均线性增长，而瞬态质量流量则持续波动，其质量流量波动幅度均呈现先减小后增大的趋势。质量流量波动幅度会受到气体工质的可压缩性与作用在毛细芯内部上的热量的共同影响。通过频谱分析发现，液相质量流量波动还会受到冷凝器两相区的影响。高热负载下，作用在毛细芯内部上的热量占主导地位，质量流量波动加剧，同时出现周期性大幅波动，且其波动频率随着热负载增大而增大。     

肠靶向海藻酸钙基微胶囊的制备及控释性能研究

利用毛细管共挤出技术结合静电吸附和仿生硅化的方法，制备了海藻酸钙-壳聚糖/精蛋白/二氧化硅(ACPSi)复合微胶囊。ACPSi复合微胶囊的平均粒径约3.18 mm，单分散性好，囊壁最外层的二氧化硅层可抑制其在肠液pH环境中的溶胀，增强囊的机械稳定性。将羟丙甲基纤维素邻苯二甲酸酯(HPMCP)肠溶微球作为释药“微阀门”，嵌入囊壁可以更好地控制微胶囊的释药行为。以吲哚美辛为模型药物，当药物浓度为22.5 mg/ml时，ACPSi载药微胶囊在pH 2.5模拟胃液中3 h时累计释药率仅为0.33%，而转移至pH 6.8模拟肠液中19 h时累计释药率为77.78%；囊壁嵌入HPMCP微球后，22 h时累计释药率可提高约4%。因此，该复合微胶囊具有良好的肠靶向作用和控释特性，作为口服肠靶向缓控释制剂具有良好的应用前景。