气相色谱-串联质谱法分析尿和血中除草剂百草枯

目的建立尿和血中百草枯的离子交换固相萃取-气相色谱-串联质谱分析方法。方法尿样加内标乙基百草枯,用732阳离子交换树脂提取;血样加内标乙基百草枯,用三氯乙酸凝聚蛋白质后取上清液用732阳离子交换树脂提取。提取物用硼氢化钠在水溶液中碱性条件下还原,还原物用有机溶剂提取进行气相色谱-串联质谱法分析。结果尿和血中百草枯的提取率分别为76％和74％,检测限分别为2ng／mL和10ng／mL,尿添加百草枯100ng／mL和血添加百草枯500ng／mL水平的回收率分别为99．6±5．6％和99．3±7．6％（Mean±CV）。结论本文建立的分析方法灵敏度高,能够满足中毒致死案件检验及临床毒物检验的需要。     

不同温度下血样中毒鼠强的稳定性

目的探讨不同保存温度下血样中毒鼠强的稳定性。方法配制毒鼠强质量浓度为0.5μg/mL的血液样品,分别置于45℃、25℃和4℃环境中保存,在配制当天及存放3、12、18和39d用气相色谱-质谱联用法测定其质量浓度,运用SPSS统计软件对结果进行统计分析。结果45℃、25℃下血样存放3d毒鼠强质量浓度基本不变,存放4～12d毒鼠强质量浓度有明显下降,存放12d后毒鼠强质量浓度缓慢下降;4℃下血样存放12d毒鼠强质量浓度基本不变,存放13～18d毒鼠强质量浓度有明显下降,存放18d后毒鼠强样品质量浓度缓慢下降。结论血样中毒鼠强质量浓度在最初的3d内稳定,此后浓度下降。保存温度对血样中毒鼠强质量浓度有影响。     

Elevated morphine concentrations determined during infant death investigations: artifacts of withdrawal of care

Abstract:  Three cases are reported of elevated postmortem blood morphine concentrations (189–3036 ng/mL) that were observed during the course of death investigations involving three children ranging in age from 1 week to 2 years, all of whom underwent withdrawal of life support. In all three cases, the presence of opiates in postmortem blood was indicated by immunoassay (ELISA) and quantitative confirmatory analysis of free morphine concentrations in postmortem blood was performed by solid-phase extraction followed by gas chromatography/mass spectrometry (GC/MS) in the selected ion monitoring mode. While the practice of withdrawing life support from terminally ill patients, with the accompanying administration of narcotics/analgesics has been reported in the medical literature, it has not been adequately described in the forensic literature. The implications of this practice on the forensic toxicological interpretation of morphine findings are discussed. To our knowledge, this is the first report of postmortem morphine concentrations arising directly from administration in conjunction with withdrawal of care in pediatric patients.     

Dominance of pre-analytical over analytical variation for measurement of methadone and its main metabolite in postmortem femoral blood

On the basis of simultaneously sampled postmortem blood specimens from the left and right femoral veins the pre-analytical variation of methadone measurements was evaluated and compared to the analytical variation. The material consisted of a series of 27 duplicate samples from routine autopsy cases comprising mainly drug addicts. A chiral LC-MS/MS method was used for measurement of the R- and S-enantiomers of methadone and its main metabolite 2-ethyl-1,5-dimethyl-3,3-diphenylpyrrolinium (EDDP). The analytical CV% was determined to be in the range 3-4% for methadone enantiomers and 4-6% for EDDP enantiomers. The total measurement uncertainty (CV(T)) was estimated from the pre-analytical variation (CV(PA)), analytical variation proper (CV(A)), and variation related to calibration (traceability) (CV(Cal)) according to the relationship CV(T) = [CV(2)(PA) + CV(2)(A) + CV(2)(cal)](0.5). Uncertainty related to calibration concerned a component related to the purity of drug reference compound and a contribution from the production of calibrator solutions (CV(Cal)<1%). Pre-analytical sampling variation was estimated from the duplicate measurements of blood samples after subtraction of the analytical component. The pre-analytical variation amounted to a CV% of 19-21% for R- and S-methadone and 30-38% for R- and S-EDDP, i.e. considerably larger than the other components. Due to the squared addition principle, the resulting total uncertainty (CV(T)) became largely identical to the CV(PA), i.e. 19-21% for R- and S-methadone and 31-38% for R- and S-EDDP enantiomers. Accordingly, CV(T) exceeded CV(A) by a factor 5 or more. Dominance of the pre-analytical component of variation may also be likely for other compounds measured in postmortem blood samples. Thus, the width of the 95%-uncertainty interval (+/-2CV(T)) for a postmortem measurement is largely determined by the pre-analytical component of variation. This should be kept in mind when judging on the uncertainty of postmortem measurement results.     

Hair analysis for cocaine: factors in laboratory contamination studies and their relevance to proficiency sample preparation and hair testing practices

Since the introduction in 2001 of a urine-based detection method for recombinant erythropoietin (rHuEPO), transfusion-doping practices have regained interest. To address this problem, an efficient antidoping test designed to obtain direct proof of allogeneic blood transfusion was developed and validated. This test, based on flow cytometry analysis of red blood cell (RBCs) phenotypes, was used to determine the absence or the presence of numerous RBCs populations in a blood sample. A such, it may constitute a direct proof of an abnormal blood population resulting from homologous transfusion. Single-blind and single-site studies were carried out to validate this method as a forensic quality standard analysis and to allow objective interpretation of real cases. The analysis of 140 blood samples containing different percentages (0-5%) of a minor RBCs population were carried on by four independent analysts. Robustness, sensitivity, specificity, precision and stability were assessed. ISO-accredited controls samples were used to demonstrate that the method was robust, stable and precise. No false positive results were observed, resulting in a 100% specificity of the method. Most samples containing a 1.5% minor RBCs population were unambiguously detected, yielding a 78.1% sensitivity. These samples mimicked blood collected from an athlete 3 months after a homologous blood transfusion event where 10% of the total RBCs present in the recipient originated in the donor. The observed false negative results could be explained by differences in antigen expression between the donor and the recipient. False negatives were more numerous with smaller minor RBCs populations. The method described here fulfils the ISO-17025 accreditation and validation requirements. The controls and the methodology are solid enough to determine with certainty whether a sample contains one or more RBCs populations. This variable is currently the best indicator for homologous blood transfusion doping.     

芦黄参花胶囊联合福辛普利治疗糖尿病肾病60例

目的 观察中西医结合疗法治疗糖尿病肾病（diabetic nephropathy,DN)的疗效及建立其综合疗效评价体系。方法 纳入Mogensen Ⅲ、Ⅳ期DN患者120例,将其随机分为治疗组（芦黄参花胶囊和福辛普利联合治疗）和对照组（单用福辛普利治疗）,疗程为3个月。比较两组的临床疗效及中医证候疗效,观察治疗前后DN患者尿白蛋白排泄率（urinary albumin excretion rate,UAER）、肾功能、血压、血糖、血脂水平,采用世界卫生组织生存质量量表简表评价患者治疗前后的生存质量。结果 对于Mogensen Ⅲ、Ⅳ期DN患者,治疗组临床疗效及中医证候疗效均显著高于对照组（P<0.05）;治疗组在降低Mogensen Ⅲ期DN患者UAER及血清肌酐、尿素氮水平,提高Mogensen Ⅲ、Ⅳ期DN患者生理健康、心理健康、总的生存质量和满意度评分方面显著优于对照组（P<0.05,或P<0.01）。两组均未见明显不良反应。结论 芦黄参花胶囊和福辛普利联合治疗可有效降低早期DN患者尿蛋白,改善肾功能,提高患者的生存质量,本研究可为DN的防治提供新的疗效评价体系。     

天舒胶囊联合西比灵治疗血瘀型偏头痛临床观察

目的 观察天舒胶囊联合西比灵治疗血瘀型偏头痛的临床疗效。方法 选择诊断为偏头痛患者60例,按序号奇偶数分成治疗组30例、对照组30例,治疗组采用天舒胶囊联合西比灵胶囊,对照组仅采用西比灵胶囊,疗程为30 d,疗程结束后1个月比较患者偏头痛积分、疼痛指数、证候积分及生活质量指数等变化。结果 两组患者偏头痛积分、疼痛指数、证候积分及生活质量指数均有显著改善,治疗组优于对照组（P<0.05）;两组患者偏头痛、疼痛、证候等疗效分布比较,差异均有统计学意义（P<0.05）,治疗组优于对照组。结论 天舒胶囊联合西比灵能显著改善血瘀型偏头痛患者的偏头痛积分、疼痛指数、证候积分及生活质量指数。     

益肾通络汤联合达英-35治疗肾虚血瘀型多囊卵巢综合征临床观察

目的 观察益肾通络汤联合达英-35治疗肾虚血瘀型多囊卵巢综合征（polycysti covary syndrome,PCOS）的临床疗效。方法 将30例肾虚血瘀型PCOS患者随机分为治疗组和对照组各15例,两组均常规给予达英-35治疗,治疗组在对照组的基础上加用益肾通络汤,疗程均为6个月。治疗前后分别检测血清雌二醇（estradiol,E2）、睾酮（testosterone,T）、促黄体生成素（luteinizing hormone,LH）、血清促卵泡素（follicle stimulating hormone,FSH）,以及空腹胰岛素（fasting insulin,FINS）水平和体质量指数（body mass index,BMI）,观察两组患者证候疗效。结果 治疗组证候疗效明显优于对照组（P＜0.05）。益肾通络汤联合达英-35能明显降低LH、T、FSH、FINS、BMI水平,提高E2水平;两组治疗前后T、LH、FSH、E2、FINS、BMI差值比较,差异均有统计学意义（P＜0.05）。治疗组改善多毛、痤疮体征的有效率均明显高于对照组（P＜0.05）。结论 益肾通络汤联合达英-35能通过调节垂体-卵巢轴相关激素水平,提高临床证候疗效,显著改善PCOS患者BMI、多毛、痤疮的体征,且安全性较好。     

金龙蛤蚧平喘胶囊治疗稳定期慢性阻塞性肺疾病临床观察

目的 观察金龙蛤蚧平喘胶囊治疗稳定期慢性阻塞性肺疾病（chronic obstructive pulmonary disease,COPD）的疗效。方法 将58例COPD患者随机分为治疗组和对照组,每组28例。在常规治疗基础上,分别给予金龙蛤蚧平喘胶囊与安慰剂。治疗前、治疗6个月后和治疗12个月后,分别观察两组患者的肺功能、骨密度（bone mineral density,BMD）、BODE指数、COPD评估测试（COPD assessment test,CAT）问卷评分及1年内急性加重次数。结果 治疗6个月后及治疗12个月后,两组肺功能各项参数比较,差异均无统计学意义（P＞0.05）。 治疗12个月后,治疗组股骨颈BMD较治疗前显著升高（P＜0.05）,而对照组股骨颈BMD较治疗前显著下降（P＜0.05）。治疗6个月后和治疗12个月后,两组BODE指数及其因子6 min步行距离积分比较,差异均有统计学意义（P＜0.05）。两组1年内急性加重次数相比,差异具有统计学意义（P＜0.05）。结论 金龙蛤蚧平喘胶囊可有效改善稳定期COPD患者的肺功能、BODE指数及生活质量,减少患者1年内急性加重次数。     

芪参护心方治疗冠心病经皮冠状动脉介入治疗术后气虚血瘀型心绞痛30例

目的 评价芪参护心方联合西药常规治疗冠心病经皮冠状动脉介入（percutaneous coronary intervention,PCI）术后气虚血瘀型心绞痛的临床疗效。方法 选取成功施行冠心病PCI术后气虚血瘀型心绞痛患者60例,随机分为对照组和研究组各30例。对照组采用阿司匹林、氯吡格雷、他汀等西药常规治疗,研究组在对照组的基础上加用芪参护心方治疗。治疗1个月后评价两组患者临床疗效、中医证候疗效及血脂变化情况。结果 研究组临床疗效、中医证候疗效均显著优于对照组（P<0.05）;治疗后两组总胆固醇、三酰甘油、低密度脂蛋白胆固醇水平均较治疗前显著下降(P<0.05),其中研究组治疗前后低密度脂蛋白胆固醇差值显著大于对照组(P<0.05)。结论 芪参护心方联合西药常规干预治疗冠心病PCI术后气虚血瘀型心绞痛有较好疗效,可明显改善心绞痛症状,减少心绞痛发生率,提高患者生活质量。