固相萃取小柱净化-气相色谱法测定蛴螬的有机氯农药残留

目的建立测定蛴螬中9种有机氯类农药残留量的方法。方法采用超声提取,固相萃取小柱净化,气相色谱法进行测定。结果所测定农药的回收率为84.0%～107.4%,样品中六六六的4种异构体、滴滴涕的4种异构体和五氯硝基苯的含量均符合国家的相关规定。结论该方法操作简便,灵敏,适用于蛴螬有机氯类农药的检测。     

GC测定山西产连翘中有机氯及拟除虫菊酯类农药残留

目的建立连翘中有机氯和拟除虫菊酯类农药残留的GC测定方法。方法样品用石油醚（60～90℃）-丙酮（4∶1）混合溶液超声提取,Florisil-氧化铝固相柱净化,用GC-ECD同时测定了9种有机氯和3种拟除虫菊酯类农药残留量。结果所测定12种农药标准曲线的相关系数r在0.999 2～0.999 9之间,回收率在80.69%～115.6%之间;17个样品（其中11个野生样品,6个栽培样品）中未检测到农药残留,3个栽培样品检测到γ-BCH和氯氰菊酯残留。结论该方法简便、快速、准确,可用于连翘中有机氯及拟除虫菊酯类农药的残留量测定;山西野生连翘生长环境优良,未受有机氯和拟除虫菊酯类农药污染。     

肉豆蔻中重金属和农药残留量分析

目的:分析中药肉豆蔻药材中重金属和有机氯农药残留量,为其质量控制和标准制定提供科学依据。方法:采用比色法测定总重金属含量,原子吸收法测定铅、镉、铜、砷的残留量,电感耦合等离子体质谱法测定汞的含量,气相色谱法测定有机氯农药六六六和滴滴涕残留量。结果:肉豆蔻药材中含总重金属小于100 mg·kg~(-1),其中铅、镉、砷、铜和汞的残留量分别为0.04～0.73,17.7×10~(-3)～85.4×10~(-3),0.01～0.09,11.0～13.5,0.06～0.34 mg·kg~(-1)。在所有样品中皆未检出滴滴涕;在某些样品中检出六六六,残留量为35.49～63.36μg·kg~(-1)。结论:肉豆蔻药材中含有一定量的重金属,其中,铜含量最高,其他重金属含量很低;10个样品中,4个样品的汞残留量稍超过国家行业标准——《药用植物及制剂进出口绿色行业标准》(2001)。所有样品中皆未检出滴滴涕,某些样品中检出六六六。     

西洋参、人参中有机氯农药残留量的快速检测

目的建立西洋参、人参中有机氯农药残留量的快速检测方法。方法用石油醚连续提取样品，采用DM-1701毛细管柱进行气相色谱测定，以外标法计算含量。结果农药六六六（BHC）、滴滴涕（DDT）、五氯硝基苯（PCNB）9个异构体均能有效分离，9个异构体在1～200μg／L质量浓度范围内与峰面积线性关系良好，r在0．9908～1．0000之间，农药残留量与药典法检测结果相符。结论该法能快速、准确、有效地测定西洋参、人参的有机氯农药残留量。     

伸筋草中重金属和农药残留量分析

目的对来自不同产地不同海拔高度的伸筋草药材中重金属和有机氯农药残留量进行分析,为控制其质量和标准制订提供科学依据。方法采用原子荧光测定砷和汞残留量,等离子体发射法测定铅和铝的残留量,气相色谱法测定五氯硝基苯(PCNB)、有机氯农药六六六和滴滴涕的残留量。结果伸筋草药材中含砷、铅、汞和铝的残留量分别为0.53～1.42,0.11～0.49,0.27～1.74 mg/kg及0.47%～1.05%。在所有样品中均未检出五氯硝基苯(PCNB),均检出微量六六六及滴滴涕。结论伸筋草药材中含有一定量的重金属,虽符合国家标准,但铝含量较高,应予以重视;所有样品农药残留量均未超过国家行业标准——《药用植物及制剂进出口绿色行业标准(2001年)》,产地不同对重金属残留有影响,但海拔高度影响不明显。产地及海拔高度对农药残留均无规律性影响。     

毛细管气相色谱法测定药物保健品中六六六、滴滴涕残留量

目的:建立药用保健品中六六六、滴滴涕残留量的毛细管气相色谱分析法。方法:采用 DB-5弹性石英毛细管(30m×0.32mm×0.5μm)色谱柱,检测器为~(63)Ni 电子捕获检测器;比较分析了3种不同前处理方法对测定六六六、滴滴涕残留量的影响。结果:六六六的4种异构体和滴滴涕的4种异构体在0.5～200ng·mL~(-1)范围内线性关系良好(r>0.9990),其检出限范围为0.024～0.53ng·mL~(-1);样品的回收率为86.2%～115.9%,RSD 为1.7%～4.7%。结论:3种处理方法中正己烷-二氯甲烷-石油醚(1:2:1)依次提取效果最好。该方法简便、快速、准确,灵敏度高,适用于同时测定药用保健品中六六六、滴滴涕8种有机氯农药残留量。     

贵州中药材GAP基地药材中有机氯农药残留的考察

目的了解贵州中药材GAP基地药材中有机氯农药残留状况。方法在贵州11个主要GAP药材基地采集中药材样品155个,采用气相色谱法检测9种有机氯农药含量。结果155个样品中有39个样品检出农药,检出率25.16%。其中六六六(BHC)、滴滴涕(DDT)、五氯硝基苯(PCNB)的检出率分别为15.48%、2.28%和5.81%。25种药材农药总残留量大小为:根系类>全草类>树皮类>茎叶类>花果类。参照《药用植物及制剂进出口绿色行业标准》,有11个样品超标,超标率为7.09%,超标的为根系类药材。结论贵州中药材GAP基地大部分药材中有机氯农药残留量低于《药用植物及制剂进出口绿色行业标准》。     

中药制剂中重金属、农药残留的监控

运用原子吸收分光光度法和气相色谱法测定了中成药制剂包括丸、片、胶囊、颗粒剂,口服液,酒剂六种不同剂型中重金属和农药残留的含量.此次随机共抽取40余品种样品,从其汇总的实验数据显示:以<中国药典>一部甘草标准项下规定重金属砷＜2mg·kg-1、汞＜0.2mg·kg-1, 有机氯农药总六六六( BHC)＜0.2 mg·kg-1 、总滴滴涕(DDT)＜0.2 mg·kg-1、五氯硝基苯(PCNB)＜0.1 mg·kg-1 限度.其中有4个品种样品中重金属砷超标,约占8%;10个品种样品的重金属汞超标,约占22%;12品种样品被检出有机氯农药残留,但低于限度标准.故对中药制剂中重金属、农药残留量的安全监控十分必要.     

西洋参、人参等药材中有机氯农药残留量的测定

目的:建立西洋参、人参等药材中分析有机氯农药六六六(BHC),滴滴涕(DDT),五氯硝基苯(PCNB)残留量的一种简便快速的毛细管气相色谱法,考察市售西洋参、人参等药材中的农药残留量情况。方法:样品用石油醚提取,以浓硫酸磺化,采用DM-1701毛细管柱(30m×0.53mm,1μm)及电子捕获检测器(ECD),外标法计算含量。结果:高、中、低3个浓度的平均加样回收率为90.41%~105.0%,RSD为0.8%~9.5%,部分样品检出的有机氯农药残留量超过国家标准。结论:建立的方法快速简便,适用于药材中有机氯农药残留量的测定。国家应尽早对西洋参和人参等根茎类药材中有机氯农药残留量制定相应的规定限量标准。     

GC法检测浙八味药材中有机氯农药的残留

目的 测定与分析白术、白芍、玄参等8种药材中9种有机氯农药残留量.方法 以混合溶剂超声提取样品、浓硫酸磺化净化,采用毛细管气相色谱,用HP-5弹性石英毛细管柱程序升温分离,微电子捕获检测器检测,峰面积外标法定量.结果 延胡索、麦冬和杭白菊均检出滴滴涕,含量分别为0.439、45.017、5.434 ng·g<'-1>;杭白菊检出五氯硝基苯,含量为1.030 ng·g<'-1>;其余药材均未检出有机氯农药残留.结论 浙八味药材大部分未检出有机氯农药残留或含量较低,均在规定的安全范围内.     

Fast pesticide multiresidue analysis in American ginseng (Panax quinquefolium L.) by gas chromatography with electron capture detection

A fast pesticide multiresidue analysis method using gas chromatography coupled with electron capture detector was investigated for the simultaneous determination of 15 organochlorine pesticides (OCPs) in American ginseng (Panax quinquefolium L.). Samples were extracted with acetic acid–water–acetonitrile (1:5:94, v/v) and cleaned up by the Quick Easy Cheap Effective Rugged and Safe multiresidue method (QuEChERS). The linearity for 15 OCPs, in the working standard solutions of seven concentration levels between 1 and 100 ng/ml, varied from 0.9990 to 0.9999. Recoveries at concentrations between 0.1 and 2 μg/g ranged from 81.4 to 95.2%, with precision, which was expressed as relative standard deviation (RSD), at values lower than 8.0%. The proposed method was applied to the determination of pesticide levels from 60 samples, taken from six different areas. Among a total of 60 samples, 15.0% (9 samples) contained at least one of the 15 pesticides. The 15 OCPs were benzene hexachloride (BHC, including α-BHC, β-BHC, γ-BHC, δ-BHC), hexachlorobenzene, heptachlor, heptachlor epoxide, aldrin, p,p′-DDE, p,p′-DDD, o,p′-DDT, p,p′-DDT, mirex, endrin and dieldrin. This study indicates that the proposed method is useful for analyzing OCPs in American ginseng.     

Levels of organochlorine contaminants in organic and conventional cheeses and their impact on the health of consumers: An independent study in the Canary Islands (Spain)

In the present work we have evaluated the levels of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in 61 commercially available brands of cheese (54 conventional and 7 organic) to estimate their relevance as a source of organochlorines. Our results showed that hexachlorobenzene, α-HCH, dieldrin, p,p′-DDE, and PCBs 153 and 180 were present in most of the samples independent of the cheese type. The concentration of OCPs was low for both types of cheese, although organic had lower concentrations than conventional. The estimated daily intake (EDI) of OCPs was lower than the tolerable daily intake (TDI). The levels of PCBs in cheese were also low; however, there were higher levels of PCBs in organic than in conventional brands. Levels of dioxin- like PCBs (DL-PCBs) in both types of cheese reached concentrations in the 75th percentile higher than 3 pg WHO–TEQ/g fat, and above 100% of the levels established by the EU. People consuming the most contaminated brands could have an EDI well above the recommended TDI (2 pg WHO–TEQ/kg bw/day). These results are of concern as the adverse health effects exerted by dioxin-like compounds are well known.     

HPLC指纹图谱鉴别滇黄芩与黄芩

目的:建立高效液相色谱指纹图谱,鉴别不同产地的滇黄芩与《中国药典》收录的黄芩。方法:采用反相高效液相色谱(RP-HPLC)法,色谱柱为Zorbax SB-C18(250mm×4.6mm,5μm),流动相为乙腈(含1.0%甲酸)-水(含1.0%甲酸),梯度洗脱,流速为1.0mL.min-1,检测波长为274nm,柱温为30℃。结果:不同产地的滇黄芩指纹图谱相似度较好,不同产地的黄芩之间指纹图谱相似度也较好;但滇黄芩与黄芩的相似度仅为0.859,存在较大差异。结论:本方法为深入研究滇黄芩与黄芩的质量标准打下了基础。     

Levels,distribution pattern and ecological risk assessment of organochlorines pesticides (OCPs) in water and sediments from two tributaries of the Chenab River,Pakistan

Residue levels, distribution patterns and ecological risk assessment of OCPs in water and sediment samples collected from two upstream feeding tributaries of the River Chenab, Pakistan were monitored. ΣOCPs levels in water and sediment ranged between 8 and 76 ng L^?1 and 17 and 224 ng g^?1, respectively. The mean concentration of ΣHCH (hexachlorocyclohexane) was 3.3 ± 3.2 ng L^?1 and 8.4 ± 9 ng g^?1 for water and sediment samples, respectively, while ΣDDT (dichlorodiphenyltrichloroethane) exhibited the average concentration of 9.07 ± 6.15 ng L^?1 and 40.3 ± 26.2 ng g^?1 for water and sediment samples, respectively. The concentration of DDT and HCHs in both water and sediment samples were about 80 % of total OCPs and DDTs were the predominant organochlorines in the investigated matrix. DDTs and HCHs in sediment samples posed higher ecotoxicological risk and results were significant when compared with the quality guidelines. Results of the present study should be taken seriously by higher authorities as there is a serious threat to ecological integrities by OCPs exposure.     

黄芩对实验性帕金森模型大鼠的保护作用

目的:研究黄芩对鱼藤酮所致帕金森(PD)模型大鼠的保护作用。方法:Wistar大鼠每日颈、背部皮下注射鱼藤酮葵花油乳化液制备PD大鼠模型;阳性组及不同剂量药物组在每日注射鱼藤酮之前1小时灌胃给药。ELISA法检测大鼠脑硫氧还蛋白(Trx);荧光探针法检测纹状体活性氧(ROS);分光光度法检测纹状体谷胱甘肽(GSH)、黑质丙二醛(MDA)含量。结果:造模后模型组大鼠出现一定程度的行为学变化,模型组Trx含量明显低于空白组、阳性组和低剂量组,药物可以一定程度上抑制氧化应激反应。结论:黄芩可以提高帕金森大鼠脑内Trx的表达,对鱼藤酮所致帕金森模型大鼠具有保护作用,这种作用可能与Trx相关。     

不同产地黄芩样品中主要有效成分含量的对比研究

目的：对不同产地黄芩样品中的主要有效成分进行对比研究。方法分别选取河北、内蒙古、甘肃三产地的黄芩样品进行分析,选用HPLC法对三组样品进行重复性、稳定性、回收率、线性关系考察及样品含量测定。结果三个产地的黄芩样品都具有很好的重复性、稳定性、回收率,黄芩样品中黄芩苷、汉黄芩苷的含量河北＞内蒙古＞甘肃,而黄芩素、汉黄芩素的含量内蒙古＞河北＞甘肃。结论不同产地的黄芩样品中的主要成分不同,在制剂中应根据不同作用选择合适产地的黄芩入药。     

Development of species sensitivity distributions and estimation of HC5 of organochlorine pesticides with five statistical approaches

Eighteen organochlorine pesticides (OCPs) were studied to develop species sensitivity distributions (SSDs) and calculate hazardous concentration thresholds for 5% of species (HC₅), using both parametric (log-normal and log-logistic) and nonparametric bootstrap methods. In order to avoid picking repetitive values in each resample when performing bootstrap, and to determine the influence of fluctuation of toxicity data of single species on the SSDs and HC₅, a modified bootstrap method was introduced, which can generate unrepetitive sampling data other than original elements in datasets. This method can enlarge a dataset without any assumption of a special distribution. Combined with parametric methods, modified bootstrap was also used to develop SSDs and determine HC₅. The HC₅ estimated by five approaches coincide well with each other with good positive correlation. Even if there is intra-species variation in a certain range of toxicity data; SSDs and HC₅ are not very sensitive to the local fluctuation of toxicity of single species. The studied OCPs were classified according to their estimated HC₅. A lower HC₅ indicates higher ecological toxicity potentials. Endrin, DDTs and Endosulfan are OCPs with very high ecological toxicity potential. α-HCH has the lowest ecological toxicity potential in the studied OCPs. For OCPs with high ecological potential, more attention should be paid to their ecological risk.     

Concentrations of organochlorine pesticides in placental tissue are not associated with risk for fetal orofacial clefts

Previous epidemiological studies have shown that prenatal exposure to organochlorine pesticides (OCPs) entails a variety of adverse impacts on fetal health, but it is not yet known whether it is associated with risk for orofacial clefts (OFCs). This study of 103 fetuses or newborns with a diagnosis of OFCs (cases) and 103 healthy newborns without malformations (controls) examined whether prenatal exposure to OCPs, as indicated by their concentrations in placental tissue, is a risk factor for OFCs. No differences were found in the median concentrations of OCPs between cases and controls, with exception of o,p’-dichlorodiphenyldichloroethylene, o,p’-dichlorodiphenyldichloroethane, and total o,p’-dichlorodiphenyltrichloroethane (DDTs), whose concentrations were higher in controls than in cases (Ps < 0.05). Although higher concentrations of placental δhexachlorocyclohexane and isodrin were found to be associated with decreased risk for OFCs in logistic regression, no association was observed in the Bayesian kernel machine regression, a novel statistical model in analyzing exposure mixtures. Women who reported periconceptional folic acid supplementation had lower placental concentrations of DDTs than women who did not. In conclusion, no association between levels of OCPs in placental tissue and risk for OFCs was observed in this population. Supplementation with folic acid may help decrease the levels of DDTs in placental tissue, but further studies are needed to confirm this unexpected finding.     

Influence of the method of production of eggs on the daily intake of polycyclic aromatic hydrocarbons and organochlorine contaminants: An independent study in the Canary Islands (Spain)

Analysis of 16 polycyclic aromatic hydrocarbons (PAHs), 20 organochlorine pesticides (OCPs) and 18 polychlorinated biphenyls (PCBs) were performed on eggs from three different production types (conventional, free-run and organic) collected from the markets of the Canary Islands (Spain). Unlike other studies we did not found differences in the content of PCBs or OCPs of eggs in relation to its production type. Median ∑OCPs content was 3.87 ng g⁻¹ fat, being dieldrin, dicofol, hexachlorobenzene, p,p′-DDE and p,p′-DDT the most frequently detected. Median ∑PCBs value was 3.93 ng g⁻¹ fat, with 79.9% of this amount coming from the marker PCBs. Two samples, one free-run and one organic, greatly exceeded the current European Commission (EC) limit of 2.5 pg TEQ_PCDD/F g⁻¹ lipid, but the rest were well below of this limit. The concentrations of PAHs in conventionally produced eggs were almost 4 times higher than in free-run or organic eggs. Mean dietary intake estimates of the organochlorine contaminants based on consumption of eggs, regardless of the type chosen, is negligible for the Canary Islands’ population. However, the median dietary intake estimates of PAHs greatly depend on the type of eggs chosen, being much lower when free-run and organic eggs are consumed.