ASE—GPC—GC—MS快速分析土壤中的PAHs

建立了土壤中多环芳烃的气相色谱—质谱联用的快速检测方法。样品经过加速溶剂萃取、凝胶色谱净化、GC—MS分离测定,优化了加速溶剂萃取和凝胶色谱净化的条件。结果表明,多环芳烃的平均回收率为82.1%~106.4%,相对标准偏差为1.2%~4.8%。方法具有灵敏度高、准确度好、快速、消耗溶剂少的优点,适用于土壤等固体样品中多环芳烃的分离、净化和分析。     

高效液相色谱法测定稻米和稻田水土中多菌灵残留

采用高效液相色谱法测定稻米和稻田水土中的多菌灵残留,用稀盐酸溶液提取,经液液分配净化,外标法定量。多菌灵的峰面积与进样质量在0．15ng-220ng范围内呈线性相关,在稻田水、土壤和稻米中的最低检出质量比分别为0．01mg／kg、0．01mg／kg和0．02mg／kg。3个质量水平的加标回收试验结果表明,多菌灵在稻田水样中的平均回收率为87．1％～93．0％,RSD为3．3％～3．8％;在土壤中的平均回收率为84．8％-91．9％,RSD为1．4％～4．1％;在稻米中的平均回收率为83．9％～89．6％,RSD为1．8％-5．5％。     

超声波提取-GC/MS法测定生物体内硝基苯类化合物

以洪泽湖中6种代表性生物为研究对象,采用超声波法提取样品中硝基苯类化合物,用凝胶色谱净化、浓缩,气相色谱／质谱联用法测定。该法与索氏提取法在同等试验条件下进行加标回收试验,前者回收率高且稳定,简便可行。方法检出限为0．008μg／g～0．030μg／g,平均加标回收率为76．5％～109％,重复测定3次的RSD为1．5％～13．0％。     

Grab and passive sampling applied to pesticide analysis in the São Lourenço river headwater in Campo Verde – MT,Brazil

In this study, the quality of surface water in the headwaters of São Lourenço River in Mato Grosso, Brazil, was evaluated in relation to contamination by pesticides. For this purpose, samples were collected between December 2015 and June 2016 by grab sampling and by passive sampling using an integrative polar organic compound sampler installed in the field during four 14-day cycles between March and June 2016. The analyses were performed by gas chromatography (CG/MS) and by liquid chromatography (UPLC-MS/MS). The results showed the detection of two pesticides (atrazine and pyraclostrobin) of the five analyzed by passive sampling and eight active principles among the 20 analyzed (malathion, diuron, carbofuran, carbendazim, trifluralin, imidacloprid, metolachlor, and acetamiprid) by grab sampling. The detection of 10 pesticides, even almost a decade after the beginning of a recovery process of the ciliary forest, confirms the headwaters' vulnerability to these contaminants and passive sampling proved to be an important tool in capturing small concentrations of pesticides constituting an interesting complement to grab sampling.     

气相色谱-串联质谱法测定沉积物中多环芳烃

采用ASE法提取沉积物中16种多环芳烃,以固相萃取法净化提取液,用气相色谱-串联质谱法测定。通过优化测定条件,使方法在5.00μg/L~1 600μg/L范围内线性良好,方法检出限为0.15μg/kg~0.66μg/kg。空白石英砂的加标回收率为61.9%~121%,7次测定结果的RSD为2.6%~11.1%。     

固相萃取-气相色谱法测定饮用水中甲基汞

根据巯基棉在一定酸性条件下能定量吸附甲基汞的原理,利用多通道并联的固相萃取装置,采用气相色谱(ECD)方法测定饮用水中痕量甲基汞,考察了水样pH值对回收率的影响.方法在0.050 mg/L～1.00 mg/L范围内线性良好,当采样体积为1.0 L时,检出限为0.03 ng/L,标准样品与实际水样平行测定的相对标准偏差均...     

固相萃取-气相色谱法测定水样中马拉硫磷残留

采用C-18小柱萃取、毛细管柱分离、气相色谱氢火焰离子化检测器（FID）测定水样中的马拉硫磷,检测限为0．12μg／L。试验了样品流量和洗脱剂对回收率的影响,结果表明样品流量为6mL／min、二氯甲烷作洗脱剂时,回收率较好。测定蒸馏水、地下水和河水样品,相对标准偏差〈2．2％。加标回收率在79．0％-109％之间。     

Pesticide residue removal in classic domestic processing of tomato and its effects on product quality

This study was undertaken to evaluate the effectiveness of several household practices (washing with water or acidic, alkaline, and oxidizing solutions, and peeling) in minimizing pesticide residue contamination of tomatoes, as well as the impact on the quality of the treated fruit. Tests were performed using two systemic fungicides (azoxystrobin and difenoconazole) and one contact fungicide (chlorothalonil). Solid-liquid extraction with low temperature partition (SLE/LTP) and liquid-liquid extraction with low temperature partition (LLE/LTP) were used to prepare the samples for pesticides determination by gas chromatography. Washing the tomatoes with water removed approximately 44% of chlorothalonil, 26% of difenoconazole, and 17% of azoxystrobin. Sodium bicarbonate (5%) and acetic acid (5%) solutions were more efficient, removing between 32 and 83% of the residues, while peeling removed from 68 to 88% of the pesticides. The washing solutions altered some fruit quality parameters, including acidity and chroma, and also caused weight loss. Acetic acid (0.15 and 5%) and hypochlorite (1%) solutions had the greatest effect on these parameters.     

盐析分相微萃取—高效液相色谱法测定水中含氯除草剂

采用盐析分相微萃取—高效液相色谱法同时测定水中3种含氯除草剂,建立并优化了反相离子对液相色谱条件,考察了萃取剂种类、盐析剂的种类和加入量及试样pH对萃取效果的影响。对氯苯氧乙酸、2,4-二氯苯氧乙酸和2,4-滴丁酯的质量浓度在0.1~100.0mg/L内与色谱峰面积呈良好的线性关系,相关系数不低于0.9992。平均回收率分别为96.29%、79.16%和70.21%,相对标准偏差小于5.3%。该方法操作简便、绿色环保,适合于水中含氯除草剂的测定。     

Risk Assessment of 26 Polycyclic Aromatic Hydrocarbon (PAH) Compounds in Parkıng Garages

The aim of this study was to determine the level of 26 polycyclic aromatic hydrocarbons (PAHs) at parking garages and to provide the necessary annual information based on occupational inhalation exposure and non-occupational inhalation exposure, which carry risks for the environment. For this purpose, 22 samples were collected continuously from both gas and particulates phase PAHs from two parking garages at Konya City Center, Turkey. The exposure-based risk of these samples was evaluated using concentrations of the carcinogenic PAH compounds. None of the 26 PAHs measured had values exceeding the recommended exposure limits (RELs) standard values for inhalation rate recommended by the World Health Organization (WHO). Exposure levels of gas and particulate PAHs for the occupational group and the public (children and adults who spend time in shopping centers) were found to be 0.07–28.24 μgm^?3 and 0.05–5.753 μgm^?3, respectively, representing levels two to four times higher than those at the control site. Maximum daily inhalation of B[a]Py was estimated at 1.33 ngd^?1 for exposure of the public and as 274 ngd^?1 for the occupational group. It is believed that traffic makes a substantial contribution to the PAH profile, which had relatively high concentrations of naphthalene (Napth) and coronene (Coro). Highly carcinogenic dibenzo(a,l)pyrene (B[al]Pyre) was found in the ambient air at two parking garages. Napth and phenanthrene (Phen) were the main compounds found in nearly all the tested samples. In this study, benzo[e]pyrene (B[e]Py) was used as a reference for PAHs because its concentration is stable and does not change seasonally. Considering the importance of these compounds in relation to human health, the aim of this work was to characterize and quantify the more toxic PAHs in parking garages. Conducting PAH sampling and their chemical analysis is very costly and labor intensive. This study produced data that can be a powerful tool for environmental forensics.