HPLC-MS/MS法快速测定鲜鱼肉中孔雀石绿及其代谢物含量

建立了鲜鱼肉中孔雀石绿及其代谢物隐色孔雀石绿残留量的高效液相色谱-串联质谱测定方法.采用电喷雾正离子模式离子化,选择反应扫描模式定量,孔雀石绿的定量监测离子对为m/z:329313,隐色孔雀石绿的定量监测离子对为m/z:331239,孔雀石绿的检出限为0.002 2ng/m L,定量限为0.007 3 ng/m L;隐色孔雀石绿的检出限为0.043 3 ng/m L,定量限为0.14 ng/m L,线性范围均为1~10 ng/m L,相对标准偏差均小于4%(n=6),方法的回收率均大于90%.     

仿Morpho蝶翅微纳结构制备及其光学特性

以Morpho Rhetenor蝴蝶鳞翅为研究对象,采用光学显微镜和电子显微镜对其蝶翅表面结构进行分析,提出一种易于操作、成本低的仿蝶翅微纳结构制备方法.以Morpho Rhetenor鳞片为生物模板,采用磁控溅射技术,借助烧结成型工艺,制备出仿蝶翅结构的Al2O3和ZnO反结构产物.再采用Rsoft软件对蝶翅结构及蝶翅样本的Al2O3和ZnO遗态结构进行光学仿真模拟,与实测的蝶翅样本反射谱进行比较.研究表明:仿真结果与所制备出的仿蝶翅微纳结构颜色及用低温原子层沉积工艺、溶胶凝胶等方法得到的结果较为近似,从而印证了该工艺的可行性,也为仿生微纳结构的制备及其应用提供了一条具有参考性的途径.     

In situ airborne virus inactivation by microwave irradiation

Infectious diseases cause tremendous costs of both human and economy annually. Previously, we have studied the bacterial, fungal, and allergen aerosol inacti- vation by direct microwave irradiation. Here, we further investigated its effects on airborne viruses. MS2 coliphage used as a human model virus was aerosolized and exposed to the direct microwave irradiation for ,-~ 2 min at three different power levels （700, 385, and 119 W）. In addition to the survival rate, the viral genes before and after the microwave treatments were also examined using PCR and gel electrophoresis. Direct exposure of airborne MS2 viruses to the microwave irradiation at 700 W for less than 2 min was shown to result in more than 90 % inactivation efficiency, about 65 % at medium power level （385 W）, and 50 % at the lowest level （119 W）. The aerosol inac- tivation rate followed a linear relationship with the microwave exposure time （R2 ---- 0.9889）. Scanning elec- tron images revealed visible damages to the viral surface after the exposure. Damages were also observed to the viral RNA genes coding for coat proteins, among which the A protein gene was completely destroyed. This study dem- onstrated that even without the filtration the direct micro- wave irradiation could also achieve rapid inactivation of viral aerosols. The information obtained can provide useful guidance on the development of microwave-based viral threat mitigation solutions in a closed or semi-closed space.     

Relationship between alanine aminotransferase levels and metabolic syndrome in nonalcoholic fatty liver disease

Objective： To investigate the relationship between alanine aminotransferase （ALT） levels and metabolic syndrome （MS） in nonalcoholic fatty liver disease （NAFLD）. Methods： A total of 26527 subjects who received medical health checkup in our hospital from January 2005 to July 2007 were enrolled in the study. The diagnosis of fatty liver was based on ultrasound imaging. MS was defined according to the criteria of the Adult Treatment Panel III. ALT, triglyceride （TG）, high density lipoprotein cholesterol （HDL-c）, fasting plasma glucose （FPG）, height, weight, waist circumference （WC）, systolic blood pressure （SBP） and diastolic blood pressure （DBP） were measured in each subject to analyze the relationship between MS and ALT activity Results： （1） The prevalence of NAFLD in men （30.94%） was significantly higher than that in women （15.65%）; （2） The incidence of MS in NAFLD （33.83%） was significantly greater than that in non-NAFLD （10.62%）; （3） Of the 6470 subjects with NAFLD, in the age-adjusted partial correlation analysis, there were statistically significant correlations between the ALT levels and most metabolic risk factors in each sex （P〈0.01）, except that ALT levels multiple stepwise regression analysis, SBP lost its significance, and had no correlation with HDL-c in women. Moreover, in the WC, body mass index （BMI）, age, DBP, TG and FPG were independently associated with ALT levels in both sexes （P〈0.05）. HDL-c remained significant and was independently related to ALT levels in men; （4） ALT levels were significantly higher in subjects with MS compared to those without MS （P〈0.001）. Mean ALT levels increased with the number of MS components in each sex （P〈0.05 for trend）. Conclusion： We found a strong relationship between ALT levels and MS in NAFLD and revealed that the cluster of MS components might be the predictor for ALT elevations.     

紫花地丁挥发性化学成分的分析

用同时蒸馏-萃取装置提取紫花地丁挥发性物质,测得紫花地丁挥发油的含量为1．65％,用GC／MS法从紫花地丁挥发油中分离并确定出36种化学成分,占挥发油总量的83．92％。用峰面积归一化法通过化学工作站数据处理系统得出各化学成分在挥发油中的相对百分含量。     

CYP3A5基因型和LC-MS/MS技术联合指导他克莫司临床个体化给药

建立他克莫司(FK506)临床个体化给药的新模式.选择活体肝移植患者2例,术前确定患者CYP3A5的基因型,并结合FK506的药代动力学参数制定初步的给药方案;给药后用高效液相色谱串联质谱检测法(LC-MS/MS)进行血药质量浓度监测,根据血药质量浓度、临床疗效、不良反应及合并用药情况调整FK506的后续给药方案.术前2例患者基因测序结果均为CYP3A5*3/*3型,属FK506慢代谢型,初始给药方案为0.045 mg·kg-1·d-1,分2次服用.给药后血药质量浓度监测结果在7.20～19.46 ng·mL-1范围;术后2例患者ALT、AST、BUN、Cr等总体均呈逐渐下降趋势,提示移植肝脏未发生急性排异反应,功能逐渐恢复;出院建议FK506剂量调整为病例1: 1 mg, 2次·d-1;病例2: 3.5 mg, 2次·d-1.2例患者应用FK506个体化给药新模式获得满意的效果,为临床合理使用FK506提供了科学的依据和方法.     

超临界CO_2萃取珊瑚姜挥发油抗部分植物病原菌活性研究

采用超临界CO_2萃取珊瑚姜挥发油,对其成分进行GC/MS分析,利用生长速率法测定珊瑚姜挥发油对水稻稻瘟、水稻纹枯及小麦赤霉病菌的抗菌活性,结果显示,珊瑚姜挥发油检出29个化学成分,含量最高的化合物为萜品烯-4-醇;珊瑚姜挥发油对小麦赤霉病菌的EC_(50)为247.80 mg/L(Y=3.7940X-4.0832,r= 0.970 5),水稻稻瘟病菌的EC_(50)为99.64 mg/L(Y=1.1651X+2.6716,r=0.9090),水稻纹枯病菌的EC_(50)为106.16 mg/L(Y=1.2878X+2.3909,r=0.9964),实验表明,珊瑚姜挥发油对供试菌株具有较强的抑制作用,显示了较好的应用开发前景。     

HPLC-MS/MS法测定盐酸拉贝洛尔中潜在基因毒性杂质

为了更好地控制盐酸拉贝洛尔中潜在的基因毒性杂质,保证用药安全,建立了高效液相色谱-质谱(HPLC-MS/MS)法检测盐酸拉贝洛尔中潜在遗传毒性杂质N-亚硝基拉贝洛尔。液相色谱条件:以Waters ACQUITY UPLC CSH C₁₈(150 mm×3.0 mm, 1.7 μm)为色谱柱,流动相A为0.01 mol/L甲酸铵-0.1%甲酸水溶液,流动相B为乙腈溶液,梯度洗脱,流速为0.5 mL/min,柱温为50 ℃,进样体积为10 μL。以电喷雾电离源为离子源,负离子模式,采用多反应监测,建立质谱条件,对盐酸拉贝洛尔中N-亚硝基拉贝洛尔进行定量检测。结果表明：N-亚硝基拉贝洛尔质量浓度在1.01~100.60 ng/mL范围内有良好的线性关系;低、中、高3个浓度的加样回收率(n=3)为96.84%~99.53%;检测限和定量限分别为0.01 ng/mL和0.03 ng/mL;6批盐酸拉贝洛尔样品中N-亚硝基拉贝洛尔的含量为0.37~0.79 ng/mL。所提出的方法灵敏度高、专属性强,可用于测定盐酸拉贝洛尔中的N-亚硝基拉贝洛尔,为盐酸拉贝洛尔的质量控制提供参考。     

污水处理中雌酮的定量分析

采用酶联免疫吸附检测(ELISA)试剂盒定量分析了某采用生物脱氮活性污泥工艺的污水厂中的原水、一级处理出水、二级处理出水、尾水和出水口下游受纳河水中的雌酮浓度,分析方法的定量检测限为0.5 ng/L.ELISA分析中增加的凝胶色谱净化步骤可降低E1检测值73.0%的假阳性,使其检测结果平均值从液相色谱一飞行时间质谱联用(HPLC-MS(TOF))的对照分析结果平均值的1.52倍降为1.15倍.ELISA分析检测值的假阳性与水样的污染程度呈正相关.     

BeH~+,BeD~+和BeT~+离子基态(X~1Σ~+)的结构与光谱常数的研究

采用单双取代耦合簇理论CCSD(T)/cc-pVQZ和二次组态相互作用方法QCISD(T)/cc-pVTZ对BeH+ ,BeD+ 和BeT+离子基态(X1Σ+)进行几何优化和单点能扫描,计算BeH+ ,BeD+ 和BeT+离子的势能曲线.利用所得势能曲线计算出相应的光谱常数(ωe,ωeχe,Be,αe和De)和分子振动能级,并与已有的实验数据进行了比较.