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841.
采用GC/ECD分析了鄱阳湖流域沉积物中有机氯农药的残留特征及生态风险,结果表明:所测样品中有机氯农药浓度范围为1.22~32.19 ng/g,其中,六六六(HCHs)、滴滴涕(DDTs)、六氯苯(HCB)在几乎所有采样点都有检出,含量分别是未检出~12.95 ng/g、0.75~12.57ng/g、未检出~10.8.所测样品中大部分W_(DDT)/(W_(DDE)+W_(DDD))>1,表明有新的DDT输入,HCHs主要为长时间降解后的农药残留.鄱阳湖流域沉积物中DDT、DDD和DDE含量绝大部分小于风险评估中值(ERM),但接近一半介于风险评估低值(ERL)和ERM之间,而且有一个点大于ERM,表明其生态风险大多介于10%~50%,但有一个点的生态风险大于50%.  相似文献   
842.
韩笑  娄喜山  张莉  王国卿  马明  王明林 《色谱》2010,28(4):341-347
建立了基质固相分散技术结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定蔬菜中苯甲酰脲类杀虫剂(除虫脲、灭幼脲、杀铃脲、氟苯脲、氟虫脲、氟啶脲、氟铃脲)和双酰肼类杀虫剂(甲氧虫酰肼、虫酰肼)的方法。蔬菜样品经中性氧化铝和石墨化炭黑研磨,乙酸乙酯淋洗,洗脱液浓缩定容后,经超高效液相色谱分离,分别在正、负离子多反应监测(MRM)模式下用电喷雾电离串联质谱测定,外标法定量。结果表明,9种杀虫剂在1~100 μg/L质量浓度范围内有良好的线性关系(R2≥0.99);在1、5、10、100 μg/kg 4个加标水平上的回收率为78.5%~112.8%;相对标准偏差为2.3%~10.2%,检出限为0.5~1.0 μg/kg。该方法操作简便快速,样品和溶剂用量少,检出限低,可满足蔬菜中苯甲酰脲类和双酰肼类杀虫剂同时检测的要求。  相似文献   
843.
土壤中有机氯农药残留分析用标准样品的制备   总被引:1,自引:0,他引:1  
介绍了土壤中有机氯农药残留分析用标准样品的制备方法。土壤样品经风干、研磨、筛分、混匀后装瓶。样品经索氏提取、弗罗里硅土小柱净化后,采用气相色谱-质谱法对残留的有机氯农药进行测定。结果表明,采自沈阳地区的土壤中的有机氯农药含量分布较为均匀,是一种理想的环境标准样品候选物样品。该研究为土壤中有机氯农药残留分析用标准样品的研制奠定了基础。  相似文献   
844.
气相色谱-串联质谱技术分析烟草中的132种农药残留   总被引:3,自引:0,他引:3  
陈晓水  边照阳  唐纲岭  胡清源 《色谱》2012,30(10):1043-1055
利用气相色谱-串联质谱(GC-MS/MS)检测技术,建立了检测烟草中的132种农药残留的高灵敏度方法。分析过程中考察了不同萃取溶剂、不同缓冲盐体系、不同净化剂对目标物回收率的影响。最终确定烟草样品以乙腈进行提取,以N-丙基乙二胺(PSA)与碳18(C18E)的混合净化剂进行净化,氮气吹近干后用正己烷-丙酮(9:1, v/v)复溶,过有机滤膜后进行GC-MS/MS测定,内标法定量。132种农药在20~2000 μg/kg之间线性关系良好(r2 >0.99);所有农药的方法定量限(LOQ, S/N=10)均低于20 μg/kg;在50、200、500 μg/kg的加标水平下,除灭蚁灵及六氯苯回收率稍低外,其他农药的平均回收率为68.10%~123.15%,相对标准偏差(RSD)为1.79%~19.88%。对国际烟草科学研究合作中心(CORESTA)2012年共同实验的烟草样品进行检测,对比本方法与已有的标准方法,其结果一致性较好。该方法准确、可靠,灵敏度好,适用于烟草中132种农药残留的快速筛查与定性、定量分析。  相似文献   
845.
沈伟健  曹孝文  刘一军  张睿  范欣  赵增运  沈崇钰  吴斌 《色谱》2012,30(11):1172-1177
建立了气相色谱-负化学源质谱检测蔬菜中17种拟除虫菊酯类农药残留量的方法。样品中的目标物经乙腈提取后,用乙二胺-N-丙基甲硅烷(PSA)和石墨化炭黑填料进行分散固相萃取净化,气相色谱-负化学源质谱选择离子监测模式测定,同位素内标法定量。在甜豌豆、绿花菜和大葱基质中均未见干扰所有农药测定的现象。17种拟除虫菊酯类农药的定量限均为0.02~5 μg/kg。在10、20、30和100 μg/kg等4个添加水平下,所有农药的回收率均为71.0%~139.0%,相对标准偏差≤12.8%。该方法可作为蔬菜中17种菊酯类农残检测的确证方法。  相似文献   
846.
对多壁碳纳米管(MWNTs)的表面进行酸氧化处理制备了改性的MWNTs,并建立了以改性MWNTs作为固相萃取(SPE)吸附剂测定农产品中痕量残留的4种有机氯农药(p,p′-DDD、p,p′-DDT、o,p′-DDT、p,p′-DDE)的SPE-高效液相色谱(HPLC)分析方法。考察了氧化处理条件、SPE操作条件和色谱条件等对有机氯农药残留测定的影响,优化了实验条件。在优化实验条件下,4种农药在较宽线性范围内线性良好,相关系数为0.9978~0.9995,检出限为0.050 mg/L;在样品中分别添加0.10、2.0、50 mg/L的4种农药,其加标回收率为78%~104%,相对标准偏差(RSD)为2.7%~7.6%。MWNTs作为SPE填料用于陈皮、西洋参、卷心菜和茶叶等样品的净化效果良好,测定结果准确,灵敏度高,符合农产品中痕量农药残留的分析方法要求,为农产品中此类农药的痕量残留分析提供了有益的参考。  相似文献   
847.
The laser diode thermal desorption (LDTD) ionization source allows ultrafast and sensitive analysis of small molecules by mass spectrometry. Signal enhancement in LDTD has been observed when coating the surface of sample microwells with a solution of ethylenediaminetetraacetic acid (EDTA) or nitrilotriacetic acid. Here we present a quantitative analysis of signal enhancement using solutions of diverse commercial proteins (lysozyme, immunoglobulin G, albumin, and fibrinogen) as coatings. Results showed that compounds with polar chemical functions such as carboxylic acid, sulfonyl, and nitro had signal enhancement factors, in most cases higher than 10, when using any of the tested proteins as coating agent. Analysis of variance revealed that immunoglobulin G and fibrinogen gave the best results. However, the signal enhancement factors obtained with these proteins were not superior to those observed with EDTA. To explain the signal enhancement effect of proteins, analysis by scanning electron microscopy of dried samples on the microwell sample plates was carried out. Images showed that salicylic acid, one of the compounds with the highest observed signal enhancement, formed a thick layer when applied directly on the uncoated surface, but it formed small crystals (<1 μm) in the presence of protein or EDTA coatings. Further crystallographic studies using powder X‐ray diffraction showed that the crystalline form of salicylic acid is modified in the presence of EDTA. Salicylic acid when mixed with EDTA had a higher percentage of amorphous phase (38.1%) than without EDTA (23.1%). These results appear to confirm that the diminution of crystal size of analytes and the increase of amorphous phase are implicated in signal enhancement effect observed in LDTD using microwell surface coatings. To design better coatings and completely elucidate the signal enhancement effect in LDTD, more studies are necessary to understand the effects of coatings on the ionization of analytes.  相似文献   
848.
Pesticides, widely applied in agriculture, can produce a variety of transformation products and their continuous use causes deleterious effects to ecosystem. Efficient and sensitive analytical techniques for enrichment and analysis of pesticides samples are highly required. Compared with other extraction methods, solid‐phase micro extraction is a solvent free, cost effective, robust, versatile, and high throughput sample preparation technique, especially for the analysis of pesticides from complicated matrices. Coupling of solid‐phase micro extraction with gas chromatography and mass spectrometry and liquid chromatography–mass spectrometry has been extensively applied in pesticide analysis. On the other hand, in recent years, combination of fast separation using solid‐phase micro extraction and rapid detection using ambient mass spectrometry is providing highly efficient pesticide screening. This article summarizes the applications of solid‐phase micro extraction coupled to mass spectrometry for pesticides analysis.  相似文献   
849.
A novel hybrid triazine‐imine core‐shell magnetic covalent organic polymer with high adsorption capacity and excellent stability was fabricated by surface‐assisted in situ growth technique. The composite possesses porous and extended π‐conjugated system, and was applied as the magnetic sorbent for efficient enrichment and rapid separation of pesticides. A new analytical method for simultaneous determination of eight pesticides in fruit samples was developed by magnetic solid phase extraction combined with ultra high performance liquid chromatography and tandem mass spectrometry. The effect of extraction time, desorption time, and the type of desorption solvent on the extraction efficiency were evaluated. The established method shows good repeatability and high sensitivity. The repeatability of this method was estimated with relative standard deviations in the range of 0.7–7.0% (n = 5) for the same batch, and 1.7–10% (n = 3) for batch to batch. Good linearity for eight pesticides was obtained with coefficient of determination in the range of 0.9942–0.9990. Limit of detections ranged from 0.4 to 1.2 ng/L. Real sample determination showed that four and two pesticides were detected in strawberry and grape, respectively. The results demonstrated that the established method was efficient, sensitive, and convenient for trace determination of pesticides in fruit samples.  相似文献   
850.
Considering that the determination of pyrethroid residues is of value for the safety of food, a new poly(ionic liquid)‐functionalized magnetic mesoporous nanoparticle was designed and used as an adsorbent in magnetic solid‐phase extraction for the enrichment of eight pyrethroids. The porous structure and large surface area of the mesoporous silica shell endow the adsorbent with abundant binding sites. In contrast to the reported poly(ionic liquids) with only one kind of functional group in the cationic part, the new poly(ionic liquids) with mixed cyano and phenyl groups in cationic part matched the chemical structure of the analytes to improve extraction efficiency. Under the optimum conditions, an effective method was established for the determination of eight pyrethroids in apples. Adsorption equilibrium can be quickly reached in 1 min, greatly decreasing the extraction time. The linearity range was found to be 10–200 ng/g, and the detection limits ranged from 0.24 to 1.99 ng/g. Recoveries of analytes in apple samples ranged from 87.3 to 119.0%, with relative standard deviations varying in the range of 3–21.2% (intraday) and 0.3–15.2% (interday). The results indicate that the proposed method is a good candidate for pyrethroid residues in apple samples.  相似文献   
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