An Enzyme-Linked Immunosorbent Assay for Determination of Dicyclanil in Animal Tissue

Dicyclanil is a toxic, pyrimidine-derived insect growth regulator used in veterinary medicine for the prevention of myiasis. A competitive indirect enzyme-linked immunosorbent assay was developed firstly for the determination of dicyclanil in animal tissue. The antigen was prepared using the glutaraldehyde method and polyclonal antibodies were obtained by immunizing rabbits with a dicyclanil-bovine serum albumin conjugate. The antibody obtained was specific for dicyclanil with an IC₅₀ of 9 ng/mL. Recoveries from sheep tissue and liquid milk were in the range of 52.5–72.4%, with coefficients of variation between 4.7% and 11.9%. The results were further confirmed by high performance liquid chromatography–tandem mass spectrometry.     

二氯苯染毒对小鼠组织中Zn、Cu、Fe含量的影响

采用亚急性试验,探讨对二氯苯（P—DCB）对小鼠组织中Zn、Cu、Fe的影响。选用36只小鼠,雌雄各半,随机分成3组,每组12只,分别给予P—DCBO（对照组）、450、900mg·kg^-1,每天灌胃染毒1次,连续7d,染毒结束后24h处死动物并称体质量、肝、肾质量,计算脏器系数。用火焰原子吸收法测定肝脏、血液和肾脏中Zn、Cu、Fe含量。与对照组相比,各染毒组体质量无明显变化。各组肝体系数无差异,但染毒组肾体系数明显高于对照组（P〈O．05）。900mg·kg^-1组肝脏中Zn含量及w（Zn）／w（Cu）值较450mg·kg^-1组有明显升高。与对照组相比,各染毒组血液中Zn含量呈现下降趋势,900nag·kg^-1组较对照组明显下降（P〈0．05）。900mg·kg^-1组肾脏中Cu质量分数明显低于450mg·kg^-1组,Fe质量分数则较对照组及450mg·kg^-1组均有降低,P—DCB可影响小鼠组织中元素Zn、Cu、Fe的含量及不同器官的再分布,提示微量元素失衡可能是P—DCB毒作用的重要机制。     

反相液相色谱-串联质谱法检测猪肝中26种β2-受体激动剂类药物残留

建立了一种猪肝中26种β2-受体激动剂药物残留的反相液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经β-葡萄糖苷酸酶/芳基硫酸酯酶酶解12 h后,加入HClO4调至pH 1,去除蛋白,残渣经过0.1 mol/L HClO4再次提取后,合并提取液,调节混合提取液至pH 4,过混合阳离子(MCX)固相萃取柱净化。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对β2-受体激动剂的定量离子和定性离子进行监测,本方法在15 min内完成26种目标化合物的分离分析。26种β2-受体激动剂在5、10和20μg/L添加水平的回收率为64.0%~112.7%,相对标准偏差小于15.2%,方法检出限为0.15~1.35μg/kg。     

晚期肝癌及肝转移癌合并腹水的治疗

晚期肝癌及肝转移癌多并发腹水,治疗较困难。作者在抗癌、纠正水电解质失衡、低蛋白血症的基础上,试用心得安、速尿治疗,观察32例病人的腹水情况,取得较好的效果。方法：32例病人常规检查,排除心脏疾患后,给予口服心得安10mg,3次/d;速尿20mg,3次/d。每天测量腹围、记录尿量,定期检查血电解质,适量补充钾,纠正低蛋白血症。连用一周,有效后继续使用至一个月,无效者停用。结果：32例病人中腹水消退6例,明显减轻15全,有效5例,无效6例,总有效率81.3%。结论：心得安、速尿联合治疗晚期肝癌及肝转移癌并发腹水,可降低门静脉高压,减轻腹水,且无特殊副作用,值得继续研究。     

Quantitative determination of paraffin oil in blood by capillary gas chromatography

A capillary gas chromatographic method is described for the quantitative determination of liquid paraffin in blood. Paraffin is extracted from blood into n-heptane. After solvent evaporation and dissolution of the residue in 100–200 μl n-heptane one μl is injected into a gas chromatograph fitted with a fused silica capillary column (Permabond® OV-1-CB-0.1, 10 m × 0.32 mm i.d.) and flame ionization detector. Analysis is performed by using an oven program [50°C (3 min)?285°C (5 min), rise 10%min]. The sensitivity (1.5 ng hexadecane) and the reproducibility prove the applicability of the method for the determination of liquid paraffin in blood and for the study of the stability of the liquid paraffin hollow fiber membranes used in an extracorporeal liver support system.     

高效液相色谱法检测六种氟喹诺酮类兽药残留前处理的优化

建立了一个检测动物源性食品中6种氟喹诺酮类药物残留的高效液相色谱方法。不同基质的样品前处理对检测影响较大:鱼、肉及肝脏等样品需经过乙腈-0.1 mol/L KH2PO4缓冲液提取,乙腈饱和的正己烷洗涤去除油脂;蛋及乳制品样品用正己烷饱和的乙腈提取,乙腈饱和的正己烷去脂。目标化合物采用高效液相色谱-荧光检测器检测,外标法定量。对市售鸡肉、猪肉、鸡蛋进行检测,添加10、20、50、100μg/kg浓度水平时,回收率在82%~105%之间,相对标准偏差在4%~12%之间,方法的检出限诺氟沙星、环丙沙星、沙拉沙星及单诺沙星为5.0μg/Kg,恩诺沙星、达氟沙星为3.0μg/Kg。     

Simultaneous extraction and clean-up of polybrominated diphenyl ethers and polychlorinated biphenyls from sheep liver tissue by selective pressurized liquid extraction and analysis by gas chromatography-mass spectrometry

We describe a selective pressurized liquid extraction (SPLE) method, followed by gas chromatography–mass spectrometry (GC–MS), for the simultaneous extraction and clean-up of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in sheep liver tissue samples. The on-line clean-up of liver tissue by SPLE was tested using differing amount of acid-modified silica (sulphuric acid:silica gel, 1:2, w/w), the most effective amount being 20 g. Different extraction solvents (iso-hexane and dichloromethane), either alone or in various combinations, were used to extract these target compounds from spiked liver samples. Variables affecting the SPLE extraction efficiency, including temperature, pressure, number of extraction cycles and static extraction time were studied; the optimum parameters were 80 °C, 10.3 MPa, 2 cycles and 5 min, respectively. The SPLE based method was compared with more traditional Soxhlet, off-line PLE, ultrasonic and heating extraction methods. Overall the mean percentage recoveries for all target chemicals using SPLE were 86–103% (n = 3, SD < 9%), and compared favourably with the Soxhlet (63–109%, n = 3, SD < 8%), off-line PLE (82–104%, n = 3, SD < 18%), ultrasonic (86–99%, n = 3, SD < 11%) and heating (72–102%, n = 3, SD < 21%) extraction methods. The limits of detection of the proposed method were 5–96 pg g⁻¹ and 2–29 pg g⁻¹ for the different PBDE and PCB chemicals studied, respectively. The outputs of the proposed method were linear over the range from 0.02 to 30 ng g⁻¹, for all PCB and PBDE congeners except for PBDE 100 and 153 (0.05–30 ng g⁻¹) and PBDE 183 (0.1–30 ng g⁻¹). The method was successfully applied to sheep liver samples for the determination of the target PBDE and PCB compounds.     

猪肝样品中莱克多巴胺测定的前处理方法

研究猪肝样品中莱克多巴胺测定的样品前处理方法。样品直接用HCl酸解并超声提取,同时添加70%~72%的高浓度HClO_4对酸解样品进行蛋白沉淀,然后经MCX固相萃取柱净化后,用液相色谱-串联质谱法检测。用正交试验考察了酸的种类、浓度、提取时间、提取温度和HClO_4体积对提取效率的影响,最佳条件为:HCl浓度为0.2mol/L,提取时间为40min,提取温度为25℃,HClO_4用量为200μL。从0.5、5.0和10.0μg/kg添加水平检测结果可以看出,方法平均回收率为82.0%~102%,日内和日间精密度4%,符合国家标准对检验方法的要求。该方法灵敏度高,精密度好,成本低,能简便、快速对样品中的莱克多巴胺进行提取,实现对动物源性食品的快速监测。     

补中益气汤对肝硬化患者机体微量元素的影响

为探讨补中益气汤对肝硬化患者机体微量元素水平的影响,采用全自动生化分析仪检测了30例服用补中益气汤肝硬化患者及30例肝硬化对照组患者血清中镁、铁、铜、锌的水平。结果表明,服用补中益气汤患者血清镁、铁、锌水平均显著高于对照组患者(P0.05),服用补中益气汤患者血清铜水平均显著低于对照组患者(P0.05)。提示了补中益气汤能显著提高肝硬化患者机体微量元素水平,对改善患者肝脏功能具有一定的作用。     

超声内镜联合CT门静脉成像技术对肝硬化GOV程度及疗效的评价

本研究探讨了超声内镜联合CT门静脉成像技术对肝硬化食管胃静脉曲张(GOV)程度及治疗效果的评价价值。选取72例肝硬化GOV患者为研究对象,根据食管静脉曲张套扎术(EVL)治疗效果分为良好组与不良组。结果发现,不良组总横断面表面积、胃左静脉、门静脉、脾静脉、肠系膜上静脉直径及门静脉长度均大于良好组,曲张静脉壁厚度小于良好组(P<0.05);总横断面表面积、胃左静脉、门静脉、脾静脉、肠系膜上静脉直径及门静脉长度与肝功能Child-Pugh分级、静脉曲张程度呈正相关,曲张静脉壁厚度与肝功能Child-Pugh分级、静脉曲张程度呈负相关(P<0.05);总横断面表面积、曲张静脉壁厚度/胃左静脉、门静脉、脾静脉、肠系膜上静脉直径及门静脉长度均为肝硬化GOV患者治疗效果的影响因素(P<0.05);超声内镜、CT门静脉成像参数联合预测肝硬化GOV患者治疗效果的AUC为0.857。可见,超声内镜、CT门静脉成像参数与肝硬化GOV程度、肝功能分级及EVL治疗效果密切相关,可为临床预测EVL治疗效果提供一定参考。