氢化物发生原子吸收法用于海藻中砷测定

建立了氢化物发生原子吸收测定微量砷的方法,分别考察了硼氢化钾浓度、体系酸度和原子化器外加电压对吸收强度的影响,在最佳条件下测定砷的线性范围为1~30μg.L-1,检出限为0.3μg.L-1,对10μg.L-1砷标准溶液进行11次测定的相对标准偏差为3.0%,方法用于海藻样品中微量砷的测定,结果满意。     

微波消解-原子荧光光谱法测定中药材中的砷

目的:建立一种聚四氟乙烯消化罐程序升温消解样品的体系,研究和确定原子荧光光谱法测定中药材中砷的方法。方法:采用聚四氟乙烯消化罐程序升温消解样品,氢化物发生-原子荧光光谱法测定中药材中的砷。结果:本方法的线性范围为0～6.0μg.L-1;r=0.9994;检出限为0.026μg.L-1;精密度为1.05%;回收率为95.4%。经与国家颁发的杨树叶标准物质同法操作核对,结果吻合。结论:该方法可广泛用于中药材中砷的测定。     

石墨炉原子吸收光谱法测定中成药中重金属的含量

目的:测定中成药银丹心脑通胶囊、金莲花胶囊和七叶安神滴丸中重金属铅、砷、镉的含量。方法:采用石墨炉原子吸收光谱法,样品消化后直接进行测定。结果:重金属铅、砷、镉的进样浓度分别在3～18、20～80、0.2～1.2μg.L-1范围内与吸光度线性关系良好,r分别为0.9996、0.9999、0.9998;3种成分的回收率在95%～103%之间。结论:上述中成药中所含铅、砷、镉含量均符合规定;本法简单、快速、灵敏,适用于中成药中微量重金属的分析。     

原子荧光光谱法测定矿物药大青盐中总砷和总汞的含量

目的研究矿物药大青盐中总砷和总汞的测定方法。方法采用湿法消解,双道原子荧光光谱法测定大青盐中的总砷和总汞。结果砷浓度在0～10μg.L-1、汞浓度在0～1.0μg.L-1范围内与原子荧光强度呈良好的线性关系,相关系数砷为0.9992、汞为0.9904,方法的检出限砷为0.0259μg.L-1、汞为0.0061μg.L-1,回收率砷为90.9%～100.8%、汞为90.0%～101.3%。结论该方法专属性强、简便易行、灵敏度高,可用于矿物药大青盐中有害元素总砷和总汞的限量控制。     

原子荧光光谱法同时测定药用玻璃容器中砷和锑的溶出量

目的:建立药用玻璃容器中砷、锑溶出量的测定方法。方法:采用断续流动进样方式,氢化物发生-原子荧光光谱法同时测定药用玻璃容器中砷、锑的溶出量。结果:砷在浓度范围为0～10.0μg.L-1内呈良好线性,r=0.999 9,检出限为0.009 0μg.L-1,平均回收率为95.08%;锑在浓度范围为0～10.0μg.L-1内呈良好线性,r=0.999 6,检出限为0.023 5μg.L-1,平均回收率为92.89%。结论:本法简便快捷,灵敏度高,专属性强,准确可靠,可作为药用玻璃容器的质量控制方法。     

原子荧光光谱法测定傣药蓬莱葛中的痕量砷和汞

目的:建立傣药蓬莱葛中砷和汞的原子荧光光谱检测方法。方法:采用氢化物发生-原子荧光分光光度法测定蓬莱葛中砷、汞的含量,并对测定方法进行方法学考察。结果:在最佳工作条件下,砷、汞的浓度与荧光强度均呈现良好的线性关系。砷的检测限为0.0148μg.L-1,RSD为≤4.0%,平均回收率为108.6%～109.7%;汞的检测限为0.1046μg.L-1,RSD≤5.7%,平均回收率为94.4%～109.0%。蓬莱葛中砷和汞元素平均含量分别为0.1537μg.g-1、0.0391μg.g-1。傣药蓬莱葛中砷、汞有害元素含量符合2010年版中国药典中有害元素的限量标准。结论:本文所用方法快速、简便、准确且灵敏度高、效果满意,为蓬莱葛中重金属含量测定提供了较好的方法。     

微波消解-石墨炉原子吸收法测定阿胶中6种微量元素含量

目的:建立阿胶中6种微量元素含量测定方法。方法:采用微波消解-石墨炉原子吸收分光光度法测定阿胶中砷、铅、铬、汞、镉、铜6种元素的含量。样品采用HNO3和H2O2进行微波消解,用石墨炉原子吸收分光光度计测定。结果:6种微量元素在其各自的浓度范围内均有良好的线性关系,相关系数均大于0.999。所测各元素的含量均低于国家标准规定的限量:砷(0.577μg.g-1)、铅(0.249μg.g-1)、铬(1.25μg.g-1)、汞(0.002μg.g-1)、镉(0.133μg.g-1)、铜(4.72μg.g-1)。结论:该方法快速简便、干扰少、精密度高,能够满足同类中药材中微量元素含量的测定。     

等离子体质谱法同时测定保健食品中多种重金属元素残留

样品经微波消解处理后,采用电感耦合等离子体质谱仪同时测定铅、砷、汞、镉、铬、镍6种重金属元素。各元素测定溶液浓度在0~8μg·L-1区间内,元素的浓度与仪器响应值之间存在良好的线性关系,相关系数均在为0.999以上;各元素不同水平加标回收率在91.7%~99.7%之间,精密度在0.56%~1.71%之间;该方法检出限均不高于1.0μg·kg-1。     

液相色谱-串联质谱法测定健康人口服复方氨酚右敏溶液后的尿药浓度

目的 建立高效液相色谱-串联质谱联用法同时测定人尿中对乙酰氨基酚和右氯苯那敏(解热镇痛药)浓度及其排泄.方法 12名健康志愿者按3×3拉丁方顺序进行,单剂口服给药后,按设计时间点收集尿样;尿样加入曲马多为内标,甲醇沉淀蛋白后进样,用多重反应监测,定量检测对乙酰氨基酚和右氯苯那敏的浓度.结果 对乙酰氨基酚和右氯苯那敏线性范围分别为0.05～20.00μg·mL-1和0.05～20.00 ng·L-1;96 h内对乙酰氨基酚和右氯苯那敏低、中、高剂量组的原形药物的平均累积排泄率分别为(3.87±0.75)%、(3.86±1.33)%、(3.56±1.45)%和(8.06±3.79)%、(7.62±3.39)%、(8.10±3.42)%.结论 本方法 适于同时测定人尿中对乙酰氨基酚和右氯苯那敏浓度,且2者在人体内主要以非原形药排泄.     

反相高效液相色谱法测定人血浆中阿立哌唑的浓度

目的:建立测定人血浆中阿立哌唑浓度的HPLC法。方法:以D iamonsilTMC18反相柱(250mm×4.6mm,5μm)为色谱柱,流动相为甲醇-0.03mol.L-1醋酸铵(90∶10),流速为0.8mL.m in-1,检测波长257nm,以乙醚为提取剂。结果:阿立哌唑的高(500μg.L-1)、中(100μg.L-1)、低(20μg.L-1)3个浓度的提取回收率分别为93.51%,93.23%,96.51%,日内、日间RSD均小于6%;分析方法的最低定量限为5μg.L-1。线性范围为5~500μg.L-1,回归方程为C=376.24F-5.48,r=0.999 7(n=9)。结论:该方法灵敏、准确、简单、快速,可用于临床血药浓度监测和药动学研究。     

原子吸收光谱法测定小活络丸中重金属的含量

目的:测定34家企业生产的小活络丸中铅、镉、砷、汞、铜的含量。方法:采用微波消解样品,石墨炉原子吸收分光光度法测定铅、镉、砷的含量;氢化物原子吸收分光光度法测定汞的含量;空气-乙炔火焰原子吸收分光光度法测定铜的含量。结果:34家企业生产的小活络丸中,铅、镉、砷、汞均有不同程度的超出规定限度。结论:该方法简单、准确,可用于小活络丸中重金属的含量测定。     

Arsenic-cadmium interaction in rats

Simultaneous exposure to cadmium and arsenic is highly probable in the urban area of San Luis Potosi, Mexico due to common localization of copper and zinc smelters. Therefore, in this work, rats were intraperitoneally exposed either to cadmium or arsenic alone, or simultaneously to both metals. The effects of these treatments on three different toxicological parameters were studied. Cadmium modified the LD50 of arsenic and conversely arsenic modified the LD50 for cadmium. At the histopathological level, arsenic appeared to protect against the cadmium effects, especially on testes. This protective effect seemed to be related to the glutathione levels found in this tissue: rats exposed to both arsenic and cadmium, presented glutathione values intermediate to those observed after exposure to either metal alone; arsenic had the highest value and cadmium the lowest. In liver, rats exposed to arsenic, cadmium or arsenic and cadmium, presented glutathione values below those in the saline group, with the lowest value corresponding to the arsenic and cadmium treatment. The results appear to support the proposed interaction between arsenic and cadmium and coexposure to both metals seems to alter certain effects produced by either metal alone.     

电感耦合等离子体质谱法测定五味治肝片中的12种元素含量

目的:测定中成药中有害元素的含量,为中成药质量安全控制提供依据。方法:采用电感耦合等离子体质谱(ICP-MS)法。射频功率1350W,采样深度8.5mm,等离子气流速15L·min-1,辅助气(高纯氩气)流速1.0L·min-1,载气(高纯氩气)流速1.14L·min-1,雾化室冷却温度1℃,雾化器为Babington,样品提升速度为0.40L·min-1。检测五味治肝片中镉、砷、铬、铜、锡、铅、锑、镍、银、锰、钡、锌元素的含量。结果:镉、砷、铬、铜、铅、锑、镍、银、锰、钡、锌检测浓度线性范围均为0.500～20.00ng·mL-1(r=0.9993～1.000),锡为0.500～10.00ng·mL-1(r=0.9998);各元素的加样回收率为95.0%～105.0%,RSD为0.3%～8.0%;样品中检出除锑、银外的所有元素,其中镉、砷、铬、铜、铅的含量均在2010年版《中国药典》规定的中药材限量范围内。结论:五味治肝片中部分元素的含量均能达到要求,但多数元素含量无相应的限量标准,锡、银、锑、镍等有害元素暂无国家限量标准,制定我国中药及其制剂中元素限量的标准具有重要意义。     

Relation between occupational exposure to lead, cadmium, arsenic and concentration of cystatin C

Lead, cadmium and arsenic represent well recognized toxic agents which in a specific manner disturb function of cardiovascular system. Cystatin C has been accepted to be a significant prognostic factor for cardiovascular diseases. The study aimed at defining relationship between occupational exposure to lead, cadmium and arsenic on one hand and concentration of cystatin C on the other. The studies were performed on 282 men occupationally exposed to lead, cadmium and arsenic. Among the tested individuals several groups of persons were distinguished: exposed exclusively to lead (Pb group), cadmium (Cd group), arsenic (As group), to lead and cadmium (Pb/Cd group), to lead and arsenic (Pb/As group) or to cadmium and arsenic (Cd/As group). In all the individuals serum concentration of cystatin C was estimated. Concentration of cystatin C was found to be significantly higher in Pb group than in Cd and As groups, also in Pb/Cd group higher than in Cd group and in Pb/As group than in As group. Positive linear correlations were established between Pb concentration in blood (Pb-B) and serum concentration of cystatin C (r=0.59; p<0.05) as well as between urinary concentration of As (As-U) and serum concentration of cystatin C (r=0.41; p<0.05). Regression analysis demonstrated that higher blood level of lead, higher urinary level of arsenic, more advanced age and higher body mass index represented independent risk factors of an increased serum concentration of cystatin C in the group of persons exposed to lead, cadmium and arsenic. Conclusions: Higher blood level of lead and higher urinary level of arsenic represented independent risk factors of an increased serum concentration of cystatin C in the group of persons occupationally exposed to lead, cadmium and arsenic. Concentration of lead in blood was significantly influencing serum concentration of cystatin C. The highest mean serum concentration of cystatin C was detected in the group of foundry workers exposed simultaneously to lead and arsenic.     

电感耦合等离子体质谱法测定丙泊酚注射液中有害元素含量

目的建立测定丙泊酚注射液中铜(Cu)、砷(As)、镉(Cd)、汞(Hg)、铅(Pb)5种有害元素含量的电感耦合等离子体质谱(ICP-MS)法。方法样品用微波消解法进行前处理,采用ICP-MS法测定,等离子体射频功率为1400W,载气为高纯氩气(流速为0.96L/min),等离子气体流速为18L/min,蠕动泵转速为0.2r/s,采样深度为7.5mm,重复次数为3次。通过在线加入内标锗、铟、铋元素来校正基体效应和干扰。结果Cu,As,Cd,Hg,Pb在各自测定范围内线性关系均良好(r≥0.9999),回收率介于91.32%~102.33%,RSD不大于3.77%(n=6)。结论该方法准确可靠、灵敏便捷,可用于丙泊酚注射液中有害元素的含量测定。     

Arsenic-cadmium interaction in rats: toxic effects in the heart and tissue metal shifts

Previously, we had shown that arsenic interacts with cadmium in rats; our results showed that the toxicity of a mixture of arsenic + cadmium cannot be predicted by the toxic mechanisms of the individual components. In this paper, we present further evidence about the interaction of arsenic and cadmium in rats. The results were: arsenic modified the 24 h-LD50 value of cadmium more clearly than cadmium did with the one of arsenic; based on the LD50 values, the mixtures we studied were more toxic than either metal alone. With single doses (As 10 mg/kg, Cd 2.6 mg/kg, and As 10 mg/kg + Cd 2.6 mg/kg) the mixture As + Cd was more toxic than each metal. At these doses, cadmium significantly induces the levels of glutathione, metallothionein, and lipid peroxidation in heart tissue, as compared to a saline group of rats. Arsenic incremented glutathione and lipid peroxidation at higher values than those obtained with cadmium. The mixture of As + Cd behaved as arsenic in the induction of lipid peroxidation and glutathione and like cadmium in metallothionein induction. Finally, rats treated with As + Cd had less Cd in liver than animals treated only with cadmium, and more As in heart tissue than rats treated only with arsenic. Our results give further evidence about the arsenic-cadmium interaction in rats, demonstrate the utility of employing different biomarkers in the study of chemical mixtures and indicate that heart tissue is affected not only by the mixture of As + Cd, but also by either metal alone.     

维生素B2注射液中镉、砷和铅的电感耦合等离子体质谱法测定

建立了电感耦合等离子体质谱法测定维生素B2注射液中的镉、砷和铅.维生素B2注射液经过微波消解,使用铟、锗、铋作为内标元素进行校正,以杨树叶为质控标准物,镉和铅在1～100 ng/ml、砷在1～150 ng/ml浓度范围内线性关系良好,回收率为92.4％～101.7％,RSD小于4.1％.     

ICP-MS法结合化学计量学用于枸杞子道地性的研究及安全性评价

目的:研究枸杞子中重金属及有害元素与道地性的相关性,并首次提出一种用于道地药材安全性评价的综合性策略.方法:该策略涵盖样品收集、分析测定、多元统计分析、安全性评价和风险评估5个步骤.样品经过微波消解后,采用电感耦合等离子体质谱(ICP-MS)法测定其重金属及有害元素的残留量,对结果进行聚类热图分析、主成分分析(PCA)...     

电感耦合等离子质谱法测定肾康注射液中重金属及有害元素

目的:建立肾康注射液中中铅、砷、汞、镉、铜5种重金属及有害元素的含量测定方法。方法:样品以微波消解后经电感耦合质谱测定,选择内标法定量以消除基体效应和干扰。结果:5种待测元素的方法检测限在0.002～0.015 mg·L-1,进样精密度RSD在1.1%～4.8%,重复性RSD在2.6%～5.6%,5种元素高、中、低3种浓度的加样回收率在103.6%～114.9%,样品溶液在消解后2 d内各元素稳定性良好。结论:方法灵敏度高,专属性好,可为监控及制订中药注射液中有害元素的限量提供参考。