不同产地冻干地黄中5种重金属及有害元素的含量测定

摘 要 目的： 用火焰原子吸收分光光度计和原子双道荧光光度计分别对不同产地冻干地黄中的Pb、Cd、Cu、As和Hg 5种重金属和有害元素进行检测。方法: 采用硝酸-高氯酸对样品进行消化后,采用原子吸收分光光度法测定Pb、Cd和Cu含量,采用原子荧光光度法测定As和Hg的含量。 结果: 各元素线性关系良好,相关系数均大于0.997 4,平均回收率为97.88%～100.90%,RSD为0.019%～4.20%（n=6）,同时发现10批样品中的4批样品部分重金属和有害元素超过《中国药典》限量标准。 结论:该方法准确度高,操作简便,快捷,适用于冻干地黄中重金属和有害元素的测定。     

血浆中铋的原子荧光光谱法测定

目的:建立了原子荧光光谱测定人血浆中铋的分析方法,为临床合理、安全用药提供依据。方法:样品经硝酸和高氯酸(5∶1)简单处理后,可直接测定。结果:方法的相对标准偏差(RSD)小于5.85%,回收率为97.00%~99.49%。结论:原子荧光光谱法可准确测定生物样品中铋的含量,方法简单、准确和快速。     

3-Year Outcomes of the OLIVE Registry,a Prospective Multicenter Study of Patients With Critical Limb Ischemia: A Prospective,Multi-Center,Three-Year Follow-Up Study on Endovascular Treatment for Infra-Inguinal Vessel in Patients With Critical Limb Ischemia

ObjectivesThis study sought to investigate the 3-year follow-up results of OLIVE registry patients.BackgroundAlthough favorable 12-month clinical outcomes after endovascular therapy (EVT) in OLIVE registry patients with critical limb ischemia (CLI) from infrainguinal disease have been reported, long-term results after EVT remain unknown.MethodsThis was a prospective multicenter registry study that consecutively enrolled patients who received infrainguinal EVT for CLI. The primary outcome was 3-year amputation-free survival (AFS), whereas secondary outcome measures were 3-year freedom from major adverse limb events (MALE), wound-free survival, and wound recurrence rate. Prognostic predictors for each outcome were also elucidated by Cox proportional hazard regression analysis or the log-rank test.ResultsThe completion rate of 3-year follow-up was 95%. Three-year AFS, freedom from MALE, and wound-free survival rates were 55.2%, 84.0%, and 49.6%, respectively. Wound recurrence out to 3 years was 43.9%. After multivariable analysis, age (hazard ratio [HR]: 1.43, p = 0.001), body mass index ≤18.5 (HR: 2.17, p = 0.001), dialysis (HR: 2.91, p < 0.001), and Rutherford 6 (HR: 1.64, p = 0.047) were identified as predictors of 3-year major amputation or death. Statin use (HR: 0.28, p = 0.02), Rutherford 6 (HR: 2.40, p = 0.02), straight-line flow to the foot (HR: 0.27, p = 0.001), and heart failure (HR: 1.96, p = 0.04) were identified as 3-year MALE predictors. Finally, CLI due to isolated below-the-knee lesion was a wound recurrence predictor (HR: 4.28, p ≤ 0.001). Three-year survival, freedom from major amputation, and reintervention rates were 63.0%, 87.9%, and 43.2%.ConclusionsIn CLI patients with infrainguinal lesions, 3-year clinical results of EVT were reasonable despite high reintervention and moderate ulcer recurrence rate. (A Prospective, Multi-Center, Three-Year Follow-Up Study on Endovascular Treatment for Infra-Inguinal Vessel in Patients With Critical Limb Ischemia [OLIVE 3-Year Follow-Up Study]; UMIN000014759)     

背角无齿蚌软体组织与养殖场水和沉积物中砷含量测定

目的:测定背角无齿蚌(Anodonta woodiana Lea)软体组织与养殖场中水、沉积物中砷的含量测定。方法:采用原子荧光分光光度法来测定背角无齿蚌养殖场中水、沉积物及体内的重金属元素砷的含量。结果:背角无齿蚌软体组织与养殖场中水、沉积物的砷含量分别为2.08 mg/kg,0.0053 mg/kg,10.04 mg/kg,养殖场沉积物中砷含量远高于背角无齿蚌软体组织的砷含量。结论:背角无齿蚌软体组织对养殖场中砷有很强的颗粒相吸收能力。     

免消解原子荧光法测定牛奶中的铅

目的:快速准确测定牛奶中的铅含量。方法:前处理采用免消解的酸蛋白沉淀,考虑到酸度对原子荧光信号的影响,在还原剂中加入弱酸,扩宽了酸度范围,同时优化了各种仪器条件,并研究了实际样品中各种阳离子的干扰。结果:该方法共检测了20份牛奶样品,检测结果与石墨炉原子吸收法对比,显示两者没有显著性差异,且三个不同水平的加标回收率在96%～103%。结论:本方法具有良好的准确性和可靠性。     

牛黄解毒片中砷元素分析

目的对牛黄解毒片中总砷、可溶性砷、可溶性砷（Ⅲ）和砷（Ⅴ）进行分析,为评价牛黄解毒片的安全性提供依据。方法采用微波消解-原子荧光法测定牛黄解毒片中的总砷含量,50%甲醇浸提-原子荧光法测定可溶性砷,717阴离子交换树脂分离-原子荧光法测定可溶性砷（Ⅲ）和砷（Ⅴ）。结果3种牛黄解毒片制剂中总砷含量为65.72～75.79g/kg,可溶性砷占总砷百分比为0.43%～1.23%,其中可溶性砷（Ⅲ）含量0.19～0.55g/kg,可溶性砷（Ⅴ）含量范围在0.09～0.44g/kg。结论不同的牛黄解毒片中可溶性砷及其中两种价态砷的含量差异较大,因此有必要对牛黄解毒片中砷的含量进行质量控制。     

高压消解-原子荧光光谱法测定食物中的汞

目的建立一种快速、简便、准确、灵敏的高压消解-原子荧光光谱法用于检测食品中的汞。方法采用硝酸/过氧化氢高压消解体系对样品进行预处理,利用原子荧光光谱法测定食品中的汞。结果在经过优化的条件下,汞的检出限为0.015μg/L,相关系数为0.999 9。样品回收率在96.8%～103.2%,相对标准偏差小于3.5%。结论该方法简便、快速、准确、灵敏度高。     

氢化物原子荧光法检测大米中汞存在的干扰及消除

目的:本文针对微波消解-氢化物原子荧光法测定大米中汞时,干扰因素的存在,如氮氧化物,亚硝酸根等,及其影响因子的消除进行了研究,优化前处理条件。方法:采用了模拟实际可能存在干扰因素的实验,并通过加入一定比例氨基磺酸后水浴的方法相关消除干扰因素。结果:分析测试汞时,就消解时溶解的氮氧化物和亚硝酸根分别进行了探讨:1μg.L-1标准溶液中一定体积亚硝酸根(0.3%m/VNaNO2)可造成90%的负偏差;酸消解过程中产生的NOx带来的干扰不固定。通过实验发现,只通过水浴消解液或在室温条件下加入氨基磺酸都不能完全恢复Hg的测试信号;但通过加入一定比例的氨基磺酸(0.3%)后,水浴1.5 h可以彻底消除上述干扰。结论:利用论文中提供的方法,可消解并分析相关的植物标准样品,可以得到满意的结果。     

消解方式对氢化物原子荧光法测定虾粉中总砷的影响

研究了三种不同消解方式——干法消解、湿法消解和微波消解,对氢化物发生原子荧光光谱法测定虾粉中微量砷的含量的影响,证明采用微波消解—氢化物发生原子荧光光谱法并不适用于虾粉中总砷的测定,只有用干法消解,或硝酸—硫酸—高氯酸湿法消解才能准确测定虾粉中的总砷。在优化实验条件下,砷的线性范围为1.0~20.0μg/L,相关系数为0.9997,样品的加标回收率为96%~107%,相对标准偏差小于10%,具有较高的测量灵敏度,稳定可靠,可应用于海产品中总砷的检测。