乳品中氨基甲酸酯类农药多残留高效液相色谱分析方法的研究

建立了乳品中氨基甲酸酯类农药（ＮＭＣＳ）多残留高效液相色谱（ＨＰＬＣ）紫外检测（ＵＶ）分析方法。采用ＯＤＳ色谱柱，确定甲醇－水（４５５５）为流动相，２１０ｎｍ下进行检测，速灭威、西维因、异丙威、呋喃丹、涕灭威等５种ＮＭＣｓ达到很好分离，分离度达２．２３以上。５种ＮＭＣｓ最低检测限为０．７５～３ｎｇ，标准曲线线性良好（ｒ＝０．９９４４～０．９９６３）。样品以丙酮提取，加入ＮａＣｌ使其饱和，再加入二氯甲烷分配，提取和分离农药一步完成。提取液再用交联聚苯乙烯凝胶（Ｂｉｏ－ＢｅａｄｓＳ－Ｘ３）净化。洗脱液为乙酸乙酯－环己烷（１１），收集流分为３５～６５ｍｌ，５种ＮＭＣｓ平均过柱回收率８６．８％～１００．０％。净化效果良好，样品添加５种ＮＭＣｓ的平均回收率在８０％以上，符合农药残留痕量分析要求。     

GC-MS分析法在人参有机氯农药残留检测中的应用

以丙酮－饱和氯化钠溶液－石油醚的一步法提取分离技术制备样品溶液,采用ＧＣ－ＭＳ分析方法对人参中有机氯农药残留进行了测定。加标人参样品的测定结果表明：两个水平加标回收率：０．１０ｍｇ／ｋｇ添加水平时,除ＰＣＮＢ平均回收率为５８．３％,其它组分的平均回收率为７６．０％～９０．１％,相对标准差为９．３％～１５．０％;０．０５０ｍｇ／ｋｇ添加水平时,平均回收率为６２．３％～８７．２％,相对标准差为６．０％～２２．５％。应用本方法测定人参中有机氯农药残留,基本上满足了灵敏、快速、准确可靠的分析方法要求     

HBV感染孕妇血清HBVM与TORCH抗体检测

目的了解ＨＢＶ感染孕妇血清ＨＢＶＭ与ＴＯＲＣＨ抗体阳性率。方法应用ＥＬＩＳＡ法筛查出９３例ＨＢＶ感染孕妇,并用ＰＣＲ检测ＨＢＶ－ＤＮＡ。分娩时取脐血测弓形体（Ｔｏｘ）、风疹病毒（ＲＶ）、巨细胞病毒（ＣＭＶ）、单纯疱疹病毒Ⅱ型（ＨＳＶ－Ⅱ）四种病原血清特异性ＩｇＭ和风疹病毒ＩｇＧ抗体。结果９３例ＨＢＶ感染孕妇中ＴＯＲＣＨ总感染率４７．３１％。单项抗体阳性率２５．８１％,７例为２项抗体阳性,２例３项抗体阳性。原发宫内感染以Ｔｏｘ最高（１２．９０％）,ＣＭＶ次之（６．４５％）,随后ＨＳＶ－Ⅱ（５．３８％）,ＲＶ最低（３．２３％）。孕妇ＨＢｓＡｇ阳性组,ＰＣＲＨＢＶ－ＤＮＡ阳性率７６．９２％,ＴＯＲＣＨ感染率６１．５４％。ＨＢｓＡｇ阴性组,ＰＣＲＨＢＶ－ＤＮＡ阳性率３８．８９％,ＴＯＲＣＨ感染率３７．０４％。结论脐血ＴＯＲＣＨ感染率与母血ＨＢｓＡｇ、ＨＢｅＡｇ、ＨＢＶ－ＤＮＡ相关（相关系数分别为０．１４、０．２９、０．１５）。乙肝感染孕妇ＴＯＲＣＨ的抗体筛查对优生优育是非常有用的指标。     

干扰素治疗丙型肝炎疗效相关因素分析

目的：探讨预测干扰素治疗慢性丙型肝炎（ＣＨＣ）疗效的临床上适用、简便、易行的指标。方法：对采用干扰素（ＩＦＮα－１ｂ）治疗３２例ＣＨＣ临床资料进行观察,包括治疗前后肝功能（ＡＬＴ、ＳＢ、ＧＧＴ）、抗－ＨＣＶＯＤ水平、ＨＣＶ基因型、ＨＣＶＲＮＡ、ＳＩＬ－２Ｒ、β２－ＭＧ等,治疗结束时有效者为肝功能复常同时ＨＣＶＲＮＡ阴转,其余反应模式均为无效者。结果：ＨＣＶ基因型为Ⅲ型患者疗效（５／１０）明显高于Ⅱ型（２／１９）（Ｐ＜０．０５）,有效者治疗前血清抗—ＨＣＶＯＤ明显低于无效者（Ｐ＜０．０５）,治疗后有效者β２－ＭＧ升高水平（３．４５±１．０８）ｍｇ／Ｌ明显高于无效者（１．３３±０．９５）ｍｇ／Ｌ（Ｐ＜０．０５）,而两者治疗前ＡＬＴ、ＳＢ、ＧＧＴ、ＩｇＭ、β２－ＭＧ患者的年龄无明显差别（Ｐ＞０．０５）。结论：感染ＨＣＶ基因型,治疗前抗—ＨＣＶＯＤ水平及治疗后β２－ＭＧ变化对预测ＩＦＮ治疗ＣＨＣ疗效有一定参考价值。     

β-胡萝卜素和核黄素对大鼠脂质过氧化的影响

目的：进一步探讨亚硝胺通过脂质过氧化而致癌的可能途径,以及研究β－胡萝卜素（β－Ｃ）和核黄素（ＶＢ２）通过抑制脂质过氧化反应而影响亚硝胺致癌的可能途径。方法：将５０只二级ＳＤ雄性大鼠随机分成５组。实验组在每日灌胃二甲基亚硝胺（ＮＤＭＮ）１．７５ｍｇ／ｋｇ的基础上,每日分别给予β－Ｃ２５ｍｇ／ｋｇ和／或ＶＢ２１８ｍｇ／ｋｇ补充,实验期为２８天。实验结束时,收集血液,摘取肝脏和肾脏,测红细胞和肝肾匀浆ＳＯＤ活性,全血ＧＳＨ－Ｐｘ活性,血清和肝肾匀浆ＭＤＡ含量,血清ＲＯＯＨ以及全血Ｈｂ含量。结果：１．ＮＤＭＮ可使ＳＯＤ和ＧＳＨ－Ｐｘ活性下降（Ｐ＜０．０５）,ＭＤＡ和ＲＯＯＨ产生增多（Ｐ＜０．０５）。２．添加β－Ｃ后,ＳＯＤ和ＧＳＨ－Ｐｘ活性有明显提高（Ｐ＜０．０５）,ＭＤＡ和ＲＯＯＨ的含量明显降低（Ｐ＜０．０５）。３．添加ＶＢ２后,肝ＳＯＤ和全血ＧＳＨ－Ｐｘ活性均有明显提高（Ｐ＜０．０５）,但ＭＤＡ和ＲＯＯＨ的含量没有差异（Ｐ＞０．０５）。４．同时补充β－Ｃ和ＶＢ２后,各项指标的变化与单纯β－Ｃ组基本一致。结论：脂质过氧化也是亚硝胺致癌的途径之一;一定剂量的β－Ｃ可对抗ＮＤＭＮ引发的脂质过氧化;核黄素对提高抗氧化?     

苦荞蛋白复合物的营养成分及其抗衰老作用的研究

分析苦荞蛋白复合物的营养成分,观察其抗衰老效果。方法：用碱抽提和等电点沉淀法从苦荞麦籽粒中制备出苦荞蛋白复合物（ＴＢＰＣ）,再用含２０％ＴＢＰＣ饲料喂小鼠,观察对小鼠血液和脏器中超氧化物岐化酶（ＳＯＤ）、过氧化氢酶（ＣＡＴ）和谷胱苷肽过氧化物酶（ＧＳＨ－Ｐｘ）的活性的影响。结果：ＴＢＰＣ的蛋白质含量为６３．４％,脂肪１２．７％,碳水化物１０．２％,灰分３．５％,粗纤维０．４％,水分９．８％。用ＴＢＰＣ饲喂后,小鼠血液、肝脏和心脏中ＳＯＤ、ＣＡＴ和ＧＳＨ－Ｐｘ活性均有不同程度提高,脂质过氧化产物丙二醛（ＭＤＡ）含量下降。结论：苦荞蛋白复合物对生物体有一定营养和抗衰老作用。     

β-胡萝卜素对二甲基亚硝胺致大鼠脂质过氧化的影响

探讨了给予二甲基亚硝胺（ＮＤＭＮ），同时补充β－胡萝卜素（β－Ｃ）后，大鼠体内抗氧化酶活性和脂质过氧化物含量的变化。结果显示，一定剂量的ＮＤＭＮ可使大鼠血红细胞、肝肾匀浆ＳＯＤ活性和全血ＧＳＨ－Ｐｘ活性下降（Ｐ＜０．０５），血清和肝ＭＤＡ和血清ＲＯＯＨ产生增多（Ｐ＜０．０５）。添加β－Ｃ（２５ｍｇ／ｋｇ）后，ＳＯＤ和ＧＳＨ－Ｐｘ活性均比单纯ＮＤＭＮ组有明显提高（Ｐ＜０．０５）。ＭＤＡ和ＲＯＯＨ含量明显低于ＮＤＭＮ组（Ｐ＜０．０５）。提示自由基和脂质过氧化反应可能也是ＮＤＭＮ及其它亚硝胺致癌的途径之一；一定剂量的β－Ｃ可对抗ＮＤＭＮ引起的自由基和脂质过氧化。     

PCR扩增IgH重排基因在检测B—NHL微小残留病中的意义

本文应用ＰＣＲ方法扩增ＩｇＨ基因重排形成的ＣＤＲ－Ⅲ序列，对１７例骨髓形态学检查正常的Ｂ细胞非何杰金淋巴瘤（Ｂ－ＮＨＬ）病人治疗前骨髓标本进行微小残留病（ＭＲＤ）检测，其中１１例Ｂ－ＮＭＬ发生ＩｇＨ基因重排（１１／１７），检出率为６４．８％，骨髓ＭＲＤ阳性的Ｂ－ＮＨＬ病人生存期明显低于ＭＲＤ阳性病人（Ｐ〈０．０５）。提示骨髓中ＲＭＤ检测可以协助估计Ｂ－ＮＨＬ病人的预后。     

维生素A缺乏大鼠红系祖细胞表面N连接型糖链结构改变的机理研究

目的：阐明维生素Ａ缺乏（ＶＡＤ）引起大鼠红系祖细胞（ＥＰＣ）表面Ｎ连接型糖链结构改变从而导致ＥＰＣ增殖分化障碍的机理。方法：经３Ｈ－甘露糖掺入和结合外切糖苷酶的系列凝集素柱层析和凝胶过滤，研究ＶＡＤ大鼠骨髓基质细胞和脾细胞条件培养液（ＢＭＳＣＭ和ＳＣＭ）对正常大鼠ＥＰＣ表面Ｎ糖链结构的影响。结果：ＶＡＤ大鼠的ＢＭＳＣＭ和ＳＣＭ可致：３Ｈ－苷露糖掺入ＥＰＣ表面Ｎ糖肽的总量减少；高甘露糖型和杂合型糖链结构比例增大，复杂型的糖链结构比例下降；而在复杂型糖链中，二天线糖链的比例和不含分叉型Ｎ－乙酰基葡萄糖（Ｂ－Ｇｎ）和核心岩藻糖（Ｃ－Ｆｕｃ）的组分降低，含Ｂ－Ｇｎ或Ｃ－Ｆｕｃ或同时含Ｂ－Ｇｎ和Ｃ－Ｆｕｃ的组分增大。结论：ＶＡＤ可能影响造血生长因子（ＩＬ－３和ＧＭ－ＣＳＦ等）的表达／活性，因而导致ＥＰＣ表面糖链的异常以及ＥＰＣ增殖分化障碍。     

腰/臀比值与糖、脂代谢相关性研究

测定２２６例ＮＩＤＤＭ、３８９例ＩＧＴ患者体质指数（ＢＭＩ）及腰／臀比值（ＷＨＲ），并与１５３例糖耐量正常对照组作了比较。结果显示：ＮＩＤＤＭ组、ＩＧＴ组ＢＭＩ、ＷＨＲ均显著高于对照组（Ｐ＜０．０１）；ＮＩＤＤＭ组ＷＨＲ显著高于ＩＧＴ组（Ｐ＜０．０１），两组间ＢＭＩ无显著性差异（Ｐ＞０．０５）。另外，ＮＩＤＤＭ组、ＩＧＴ组的ＦＩｎｓ、２ｈＢＧ、２ｈＩｎｓ、ＴＧ、ＳＢＰ、ＤＢＰ及高血压患病率均显著高于正常组（Ｐ＜０．０１）；ＮＩＤＤＭ组ＦＢＧ、ＦＩｎｓ、２ｈＢＧ、ＴＧ及高血压患病率显著高于ＩＧＴ组（Ｐ＜０．０１），而ＩＤ１、２ｈＩｎｓ、ＩＤ２显著低于ＩＧＴ组（Ｐ＜０．０１）。ＮＩＤＤＭ组Ｃｈ明显高于对照组（Ｐ＜０．０５），而ＩＧＴ组Ｃｈ与对照组相比无显著性差异（Ｐ＞０．０５）。相关分析结果示ＷＨＲ与ＩＤ１、ＩＤ２、Ｃｈ、ＴＧ、ＳＢＰ、ＤＢＰ，均呈正相关。提示ＷＨＲ是体脂分布对糖、脂及胰岛素代谢影响较重要的指标。     

Perinatal metabolism of dichlorodiphenyldichloroethylene in Nicaraguan mothers.

Umbilical cord and venous blood samples were collected at the time of delivery from 52 mothers living in urban and rural areas of the Atoya River basin, Nicaragua. In a subsample of 24 mothers that delivered by Cesarean section, abdominal adipose tissue samples were also collected, as was breast milk later in lactation. Cord and venous blood sera were analyzed for 13 organochlorine pesticides: 1,1,1-trichloro-2,2-bis(4-chlorophenyl)ethane (pp'-DDT); 1,1-dichloro-2,2-bis(p-chlorophenyl)ethylene (pp'-DDE); pp'-dichlorophenyldichlorodiene (pp'-DDD); alpha-hexachlorocyclohexane (alpha-HCH); beta-hexachlorocyclohexane (beta-HCH); gamma-hexachlorocyclohexane (gamma-HCH); delta-hexachlorocyclohexane (delta-HCH); toxaphene; dieldrin; endrin; aldrin; heptachlor; and heptachlor epoxide. In venous blood only pp'-DDE (100% of samples), pp'-DDT (1.92%), dieldrin (15.38%), heptachlor (15.38%), gamma-HCH (7.69%), beta-HCH (11.53%), and delta-HCH (1.92%) were found, whereas in cord blood only pp'-DDE (100%), pp'-DDT (3.84%), dieldrin (19.23%), and heptachlor (9.16%), were found. The persistent DDT metabolite pp'-DDE, present in all samples of blood serum, adipose tissue, and breast milk, was studied in relation to maternal characteristics such as body mass index (BMI), age, lactation experience, and fetal pesticide acquisition. Mean venous (7.12 microg/g) and cord (6.39 microg/g) pp'-DDE concentrations were not significantly different but were significantly correlated. pp'-DDE in maternal adipose tissue was positively correlated with pp'-DDE in cord blood (P=0.0001) and breast milk (P<0.0001) and marginally correlated with changes in BMI (r=-0.03088; P=0.06). There was a higher proportion of samples (58%) with a greater concentration of DDE in venous than in cord blood. Although DDE accumulation may be less during fetal development than during breast feeding, exposure during embryogenesis may be more important than during the postnatal period.     

Organochlorine Pesticide Residues in Sediment Cores of Sunderban Wetland, Northeastern Part of Bay of Bengal, India, and Their Ecotoxicological Significance

This paper presents the first comprehensive report of the organochlorine pesticide residues (OCs) such as hexachlorocyclohexane isomers (HCHs), dichlorodiphenyltrichloroethane and its six metabolites (DDTs), and hexachlorobenzene (HCB) in core sediments (<63-μm particle size) from the Indian Sunderban wetland. The pooled mean values of the mass fraction of ΣHCHs, HCB, and ΣDDTs in the sediments were 0.05–12, 0.05–1.4, and 0.05–11.5 ng g⁻¹ dry weight, respectively. The vertical distribution of pesticides reveals an erratic pattern. The concentration of four isomers of HCHs reveals a heterogenic distribution where γ-HCH (lindane) and β-HCH shared the dominant part. The mass fraction of HCB did not show any sharp spatial variation. The prevailing sequence of DDT metabolites indicates an active degradation of the parent compound in the sediments and/or inputs of already degraded pp’DDT to the region. Peak concentrations of HCH isomers and DDT metabolites have the potential to induce ecotoxicological impact as per the sediment quality guidelines.     

Bio-monitoring of Persistent Organochlorines in Human Milk and Blood Samples from Sub-Himalayan Region of India

In the present study, concentrations of organochlorine pesticide residues viz. Dichlorodiphenyltrichloroethane and its metabolites (DDTs) and Hexachlorocyclohexane isomers (HCHs) in human breast milk and human blood samples, collected from several high altitude regions of Garhwal Himalaya in Uttarakhand, India viz. Devprayag, Chamoli, Uttarkashi, Joshimath, Bhatwari and Gangnani (altitude ranging from 472 to 1,982 m above sea level) were determined. Mean concentrations of HCH and DDT in human milk samples ranged from 4.53 to 34.32 mg/kg and 6.09 to 12.98 mg/kg, respectively. While the human blood showed mean values ranging from 6.64 to 281.7 μg/L and 12.37 to 104.10 μg/L for HCH and DDT, respectively. The study showed much higher concentrations of organochlorine residue contamination in the Garhwal region as compared to other parts of India. Risk assessments for infants were also calculated and were found within WHO limits.     

Organochlorine pesticide residues in tea

Organochlorine pesticides still exist as environmental pollutants in many countries. In this paper, the results of monitoring of organochlorine pesticides in teas taken from the Polish market in 1998 year are presented. The monitoring included analysis of organochlorine insecticides and their metabolites (sigma DDT, sigma HCH, HCB, Heptachlor, Epoxide heptachlor, and Aldrin) in samples of black and green tea, and fruit tea. The mean concentration of the organochlorine compounds in the black tea ranged from 0.0002 to 0.003 mg/kg of product, and in the green and fruit teas from 0.0001 to 0.003 mg/kg of product depending on the pesticide. In no case the violation of the Maximum Residues Limits was observed. The results obtained in this monitoring did not differ from the results reported by the other authors.     

Evaluation of organochlorine pesticides in serum from students in Coimbra, Portugal: 1997-2001

In 1997, 1999, 2000, and 2001, in an attempt to evaluate the contamination level of a Portuguese population, organochlorine pesticide residues were evaluated in human serum from students of the University of Coimbra. Concentrations of selected organochlorine pollutants (alpha-, beta-, and gamma-HCH, aldrin, dieldrin, HE, HCB, p,p'-DDT, o,p'-DDT, p,p'-DDE, p,p'-DDD) and endosulfan sulfate was measured with gas chromatography-electron capture detector. Our objective is to point out the general levels of pesticide contamination and the differences between the four populations; and together with this, if a connection could be established with gender or the residence area of the subjects. Endosulfan sulfate, p,p'-DDE, o,p'-DDT, and p,p'-DDD were the most frequently identified residues. Endosulfan sulfate present the highest concentrations for all subjects, 42.6 microg/l, with concentrations ranging from undetected to 1295.5 microg/l. Between DDT, isomers, and analogues, o,p'-DDT, and p,p'-DDT presented the highest levels, 24.8 and 21.9 microg/l, respectively. Mean total DDT levels were higher than mean total HCH levels. For summation operator-DDT, the highest levels were found among female gender and urban samples. An opposite situation was found in summation operator-HCH: males presented higher levels than females. The mean concentration of organochlorine pesticide residues, present in the student populations, showed that it is among the highest levels of contamination, when compared with others from Europe, Asia, and America.     

Organochlorine Pesticide Residues in Bovine Milk from Organic Farms in Chiapas,Mexico

Thirty six samples of bovine milk were collected from Chiapas State, Mexico between January 2011 and December 2011 with the intention of identifying and quantifying organochlorine pesticide residues in organic farms. The analyses were done using gas chromatography with an electron capture detector (Ni⁶³). In general the values found in raw milk were lower than the permissible limit proposed by FAO/WHO/Codex Alimentarius 2006. Average concentrations for alpha + beta HCH were 3.62 ng/g, gamma HCH 0.34 ng/g, heptachlor + epoxide 0.67 ng/g, DDT and isomers 1.53 ng/g, aldrin + dieldrin 0.77 ng/g, and endrin 0.66 ng/g (only present in samples from farm 2). The organic milk from Chiapas has shown low concentrations of pesticide residues in recent years and satisfies international and national regulations for commercialization.     

Organochlorine Pesticide and Polychlorinated Biphenyl in Feathers of Resident and Migratory Birds of South-West Iran

Persistent organochlorine pesticides (OCPs), such as dichlorodiphenyltrichloroethane (DDT) and its metabolites, hexachlorobenzene (HCB), α-, β-, and γ-hexachlorocyclohexane (HCH) isomers, together with polychlorinated biphenyl (PCB) congeners (IUPAC Nos. 28, 52, 101, 138, 153, and 180) were determined in tail feathers from 35 birds belonging to 15 species, all originating from the southwest of Iran (Khuzestan, coast of the Persian Gulf) and kept in museum collections. The patterns of organochlorine contaminants (OCs) in birds varied depending on their migratory behavior. Resident birds contained higher median PCB concentrations (<LOQ-151 ng/g feather) than HCHs, DDTs, and HCB. Locally migrating birds had higher median concentrations of HCHs (19–83 ng/g feather). In contrast, long-distance migrants had lower concentrations of HCB and HCHs. A positive correlation was observed among OCs in these birds, suggesting that trophic level, feeding strategy, and taxonomic group are influencing factors for the OC concentrations in bird feathers. An estimate of the risk associated suggests that levels of OCPs and PCBs were lower or close to the threshold reported to affect reproduction in 1990s.     

Organochlorine pesticides in freshwater fish from the Zagreb area

The aim of this study was to determine the level of organochlorine pesticides in freshwater fish from the Zagreb area, Croatia. The study included 215 freshwater fish samples from three sites: the Sava River, Lake Jarun, and five fishponds from the Zagreb surroundings. Organochlorine pesticides DDT and derivates, HCH, HCB, lindane, aldrin, dieldrin, endrin, heptachlor with epoxide, and methoxychlor were determined using the GC-ECD method. The determined amounts of organochlorine pesticides were within allowed concentration limits in all analysed fish samples. Median values ranged from below the detection limit of 0.01 microg kg(-1) for dieldrin and metoxychlor to 2.00 microg kg(-1) for DDT in the Cyprinidae fish family from the Sava River, Zagreb sampling site (group 1).This study has confirmed pesticide persistence in the overall ecosystem in our country despite the ban of some thirty years ago, like in many other parts of the world.     

Transport of organochlorine residues in the rat and human blood

Organochlorine residues (OCR)² are poorly soluble in water and are transported in the organism bound by the blood components. The distribution among blood fractions (cells/plasma, lipoproteins/rest of plasma proteins) were variable depending on the residue (HCB,p p-DDE, HCH, Aroclor^® 1260, PCP) and on the species (rat, man). Differences were not found betweenin vivo (after oral single dosing) andin vitro (blood incubation) experiments. Results indicated a high affinity of organochlorine residues for lipo-proteins; however, binding to blood carriers was very weak as demonstrated by the rapid release of residues by elution through a reverse phase column. The effects of residue binding to blood components on the distribution kinetics to tissues are discussed.Abbreviations CM chylomicrons - CMC carboxymethyl cellulose - DDE dichlorodiphenyl dichloroethene - HCB hexachlorobenzene - HCH hexachlorocyclohexane - HDL high density lipoproteins - LDL low density lipoproteins - OCR organochlorine residues - PCBs polychlorinated biphenyls - PCP pentachiorophenol - VLDL very low density lipoproteins