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A sensitive solid-phase microextraction/gas chromatography-based procedure for determining pentachlorophenol in food. 基于固相微萃取/气相色谱的食品中五氯酚测定方法。
Pub Date : 2007-07-01 DOI: 10.1080/02652030701216735
Natalia Campillo, Rosa Peñalver, Manuel Hernández-Córdoba

A new method for the determination of pentachlorophenol (PCP) in different foods was developed using capillary gas chromatography (GC) and microwave induced-plasma atomic emission spectrometry (MIP-AED). The analyte is first derivatized and then extracted and pre-concentrated by solid-phase microextraction (SPME) in headspace (HS) mode. A clear matrix effect was found for the different samples investigated, so that standard addition was required for quantification. Detection limits of 0.03-6.0 ng g(-1) were obtained, depending on the sample analysed. The method gave recoveries of 81-109% from spiked samples. Concentration levels of PCP ranged from 0.3 to 1.5 ng g(-1) were found in honey, but no PCP was detected in other samples.

建立了毛细管气相色谱-微波诱导等离子体原子发射光谱法测定不同食品中五氯酚(PCP)的新方法。分析物首先衍生化,然后在顶空(HS)模式下通过固相微萃取(SPME)进行萃取和预浓缩。不同样品间存在明显的基质效应,定量时需加入标准品。根据所分析的样品,获得0.03-6.0 ng g(-1)的检出限。该方法加样回收率为81 ~ 109%。蜂蜜中PCP的浓度范围为0.3至1.5 ng g(-1),但其他样品中未检测到PCP。
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引用次数: 5
Organochlorine and organophosphate pesticide residues in wheat varieties from Serbia. 塞尔维亚小麦品种中有机氯和有机磷农药残留。
Pub Date : 2007-07-01 DOI: 10.1080/02652030601182888
B Skrbić

A survey was carried out to assess the levels of 20 organochlorine and 15 organophosphate pesticides in wheat grown in two regions of the Vojvodina Province in Serbia. A total of 49 samples of seven wheat varieties were collected during the 2004 harvest. In addition, a composite sample of cultivated wheat varieties was prepared from 36 samples coming from the same regions harvested in 2003 for comparison. Official method of analysis AOAC 970.52 was applied for the determination of pesticide residues. The ranges of mean values for organochlorine residues were 32-47 ng g(-1) for beta-HCH; 28-41 ng g(-1) for gamma-HCH; <1-61 ng g(-1) for aldrin; 5-132 ng g(-1) for dieldrin; 15-111 ng g(-1) for endrin ketone; and <1-77 ng g(-1) for endrin aldehyde. For organophosphate residues the ranges were: 7-27 ng g(-1) for thionazin; <5-35 ng g(-1) for disulphoton; 42-79 ng g(-1) for parathion methyl; 422-1336 ng g(-1) for chlorpyriphos; and <5-281 ng g(-1) for parathion. The mean levels of residues were compared with the regulated maximum levels according to the European Commission and Serbian national regulation, and the average intake of residues from wheat-based products was estimated for the Serbian population.

开展了一项调查,以评估在塞尔维亚伏伊伏丁那省两个地区种植的小麦中20种有机氯和15种有机磷农药的含量。2004年收获期间共采集了7个小麦品种的49个样品。此外,从2003年同一地区收获的36个小麦品种样品中制备了一个复合样品进行比较。农药残留量测定采用AOAC 970.52国标分析方法。有机氯残留量的平均值为32 ~ 47 ng g(-1);γ - hch为28-41 ng g(-1);
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引用次数: 20
Optimisation of a sample preparation procedure for the screening of fungal infection and assessment of deoxynivalenol content in maize using mid-infrared attenuated total reflection spectroscopy. 中红外衰减全反射光谱法筛选玉米真菌感染及评估脱氧雪腐镰梨醇含量的样品制备工艺优化
Pub Date : 2007-07-01 DOI: 10.1080/02652030601186111
Gregor Kos, Hans Lohninger, Boris Mizaikoff, Rudolf Krska

A sample preparation procedure for the determination of deoxynivalenol (DON) using attenuated total reflection mid-infrared spectroscopy is presented. Repeatable spectra were obtained from samples featuring a narrow particle size distribution. Samples were ground with a centrifugal mill and analysed with an analytical sieve shaker. Particle sizes of <100, 100-250, 250-500, 500-710 and 710-1000 microm were obtained. Repeatability, classification and quantification abilities for DON were compared with non-sieved samples. The 100-250 microm fraction showed the best repeatability. The relative standard deviation of spectral measurements improved from 20 to 4.4% and 100% of sieved samples were correctly classified compared with 79% of non-sieved samples. The DON level in analysed fractions was a good estimate of overall toxin content.

介绍了用衰减全反射中红外光谱法测定脱氧雪腐镰刀菌醇(DON)的样品制备方法。从粒度分布较窄的样品中获得了可重复的光谱。样品用离心磨粉机磨碎,用分析筛振动筛分析。的粒径
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引用次数: 26
Determination of acrylamide in coffee and chocolate by pressurised fluid extraction and liquid chromatography-tandem mass spectrometry. 加压流体萃取-液相色谱-串联质谱法测定咖啡和巧克力中的丙烯酰胺。
Pub Date : 2007-07-01 DOI: 10.1080/02652030701235198
O Pardo, V Yusà, C Coscollà, N León, A Pastor

A selective and sensitive procedure has been developed and validated for the determination of acrylamide in difficult matrices, such as coffee and chocolate. The proposed method includes pressurised fluid extraction (PFE) with acetonitrile, florisil clean-up purification inside the PFE extraction cell and detection by liquid chromatography (LC) coupled to atmospheric pressure ionisation in positive mode tandem mass spectrometry (APCI-MS-MS). Comparison of ionisation sources (atmospheric pressure chemical ionisation (APCI), atmospheric pressure photoionization (APPI) and the combined APCI/APPI) and clean-up procedures were carried out to improve the analytical signal. The main parameters affecting the performance of the different ionisation sources were previously optimised using statistical design of experiments (DOE). PFE parameters were also optimised by DOE. For quantitation, an isotope dilution approach was used. The limit of quantification (LOQ) of the method was 1 microg kg(-1) for coffee and 0.6 microg kg(-1) for chocolate. Recoveries ranged between 81-105% in coffee and 87-102% in chocolate. The accuracy was evaluated using a coffee reference test material FAPAS T3008. Using the optimised method, 20 coffee and 15 chocolate samples collected from Valencian (Spain) supermarkets, were investigated for acrylamide, yielding median levels of 146 microg kg(-1) in coffee and 102 microg kg(-1) in chocolate.

开发并验证了一种选择性和敏感的方法,用于测定咖啡和巧克力等难处理基质中的丙烯酰胺。该方法包括乙腈加压流体萃取(PFE)、PFE萃取池内florisil净化净化和液相色谱(LC)耦合常压电离正模串联质谱(APCI-MS-MS)检测。比较了电离源(大气压化学电离(APCI)、大气压光电离(APPI)和APCI/APPI组合)和净化程序,以改善分析信号。影响不同电离源性能的主要参数先前使用实验统计设计(DOE)进行了优化。通过DOE对PFE参数进行了优化。定量时采用同位素稀释法。该方法的定量限(LOQ)分别为咖啡1 μ g kg(-1)和巧克力0.6 μ g kg(-1)。咖啡和巧克力的回收率分别为81-105%和87-102%。准确度采用咖啡参考测试材料FAPAS T3008进行评估。利用优化后的方法,对从西班牙巴伦西亚超市收集的20份咖啡和15份巧克力样品进行了丙烯酰胺检测,结果显示,咖啡和巧克力的丙烯酰胺中位数分别为146微克/千克和102微克/千克。
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引用次数: 24
Phytosterol consumption and the anabolic steroid boldenone in humans: a hypothesis piloted. 植物甾醇消耗和人类合成代谢类固醇胆甾酮:一个假设试点。
Pub Date : 2007-07-01 DOI: 10.1080/02652030701216727
M M Ros, S S Sterk, H Verhagen, A F H Stalenhoef, N de Jong

The presence of the anabolic steroid boldenone in animals has become a research topic as its occurrence is proposed to be a marker for illegal hormone administration. However, boldenone can also be formed from beta-sitosterol, a phytosterol present in animal feed, as well as from endogenous sources. The observations in animals together with the increased consumption of phytosterol-enriched foods in the Western population led the authors to the hypothesis that consumption of phytosterol-enriched foods might possibly lead to increased boldenone levels in humans. The authors performed a pilot study among female volunteers (n = 10) to investigate whether boldenone concentrations in urine were detectable after consumption of 25 g day(-1) of phytosterol-enriched margarines for 1 week. Urine samples were collected at days 0, 3 or 4, and 7. Urine of a sitosterolemia (a rare autosomal recessively inherited lipid metabolic disorder) patient was collected as a positive control case. No traces of boldenone were detected in either the volunteers or in the patient. In conclusion, there is no evidence of formation of boldenone in women after consumption of the recommended amount of phytosterol-enriched margarines.

合成代谢类固醇胆甾酮在动物体内的存在已成为一个研究课题,因为它的出现被认为是非法使用激素的标志。然而,也可以由-谷甾醇(动物饲料中的一种植物甾醇)以及内源性来源形成胆甾酮。通过对动物的观察,再加上西方人群中富含植物甾醇的食物摄入量的增加,作者提出了这样的假设:食用富含植物甾醇的食物可能会导致人类体内胆甾醇含量的增加。作者在女性志愿者(n = 10)中进行了一项初步研究,以调查在连续一周每天食用富含植物甾醇的人造黄油25克后,尿液中的胆甾酮浓度是否可以检测到。于第0、3、4、7天采集尿样。收集1例谷甾醇血症(一种罕见的常染色体隐性遗传脂质代谢紊乱)患者尿液作为阳性对照病例。在志愿者和病人身上都没有检测到波地酮的痕迹。总之,没有证据表明,在食用了推荐量的富含植物甾醇的人造黄油后,女性体内会形成胆甾酮。
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引用次数: 19
Analysis of polycyclic aromatic hydrocarbons in vegetable oils combining gel permeation chromatography with solid-phase extraction clean-up. 凝胶渗透色谱与固相萃取净化相结合分析植物油中的多环芳烃。
Pub Date : 2007-07-01 DOI: 10.1080/02652030601150505
A Fromberg, A Højgård, L Duedahl-Olesen

A semi-automatic method for the determination of polycyclic aromatic hydrocarbons (PAHs) in edible oils using a combined gel permeation chromatography/solid-phase extraction (GPC/SPE) clean-up is presented. The method takes advantage of automatic injections using a Gilson ASPEC XL sample handling system equipped with a GPC column (S-X3) and pre-packed silica SPE columns for the subsequent clean-up and finally gas chromatography-mass spectrometry (GC-MS) determination. The method was validated for the determination of PAHs in vegetable oils and it can meet the criteria for the official control of benzo[a]pyrene levels in foods laid down by the Commission of the European Communities. A survey of 69 vegetable oils sampled from the Danish market included olive oil as well as other vegetable oils such as rapeseed oil, sunflower oil, grape seed oil and sesame oil. Levels of benzo[a]pyrene in all the oils were low (<0.2-0.8 microg kg(-1)), except for one sample of sunflower oil containing 11 microg kg(-1) benzo[a]pyrene.

建立了一种凝胶渗透色谱/固相萃取(GPC/SPE)联合净化的半自动测定食用油中多环芳烃(PAHs)的方法。该方法利用了Gilson ASPEC XL样品处理系统的自动进样优势,该系统配备了GPC柱(S-X3)和预填充二氧化硅固相萃取柱,用于随后的清理和最后的气相色谱-质谱(GC-MS)测定。该方法经验证可用于植物油中多环芳烃的测定,符合欧共体委员会制定的食品中苯并[a]芘的官方控制标准。一项从丹麦市场取样的69种植物油的调查包括橄榄油以及其他植物油,如菜籽油、葵花籽油、葡萄籽油和芝麻油。所有油中苯并[a]芘的含量都很低(
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引用次数: 90
Analysis of risk assessment and risk management processes in the derivation of maximum levels for environmental contaminants in food. 食品中环境污染物最高限量推导过程中的风险评估和风险管理过程分析。
Pub Date : 2007-07-01 DOI: 10.1080/02652030701216701
Klaus Schneider, Inga Ollroge, Martin Clauberg, Ulrike Schuhmacher-Wolz

Environmental contaminants originate from diverse sources and, owing to their ubiquitous presence in the environment, may appear in foods. Setting standards in food is increasingly important within the European Union and world-wide to protect consumers' health and to avoid trade barriers. This paper analyses how maximum levels for environmental contaminants in food were derived by the Codex Alimentarius Commission, by the European Union and by national authorities (USA, Germany). Both the risk assessment process (derivation of tolerable intake values and intake assessment by scientific bodies) and the risk management process (derivation of maximum levels by risk management bodies) are discussed. The various organizations show similar approaches and similar numerical values for maximum levels of the same contaminants in the same food items. In the area of decision-making for risk management, there was a noticeable lack of transparency in all the investigated systems. Recommendations are made for the development and harmonization of exposure assessment and communications between risk assessment and risk management processes, for improvements in documentation and for greater transparency within risk management decision-making processes.

环境污染物的来源多种多样,由于它们在环境中无处不在,可能会出现在食品中。在欧洲联盟和世界范围内,制定食品标准对于保护消费者健康和避免贸易壁垒越来越重要。本文分析了食品法典委员会、欧盟和国家当局(美国、德国)如何得出食品中环境污染物的最高水平。讨论了风险评估过程(科学机构确定可容忍摄入量和摄入量评估)和风险管理过程(风险管理机构确定最高水平)。不同的机构对相同食品中相同污染物的最大含量给出了相似的方法和数值。在风险管理决策领域,所有被调查的系统都明显缺乏透明度。建议制定和统一风险评估以及风险评估和风险管理过程之间的沟通,改进文件,提高风险管理决策过程的透明度。
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引用次数: 9
Clostridium perfringens and its toxins in minced meat from Kars, Turkey. 土耳其卡尔斯肉糜中的产气荚膜梭菌及其毒素。
Pub Date : 2007-07-01 DOI: 10.1080/02652030601186129
U Kamber, H I Gokce, M Elmali

The aim of this study was to determine the prevalence of Clostridium perfringens and its toxins in minced meat. A total of 96 minced meat samples were collected from local markets (16) and small butcher's shops (80) in Kars (Turkey). Samples were analysed for the presence of C. perfringens and its toxins using a commercially available ELISA kit. A total of 31 (32%) Clostridium spp. strains were isolated and 17 (55%) of these isolates were identified as C. perfringens. Four (25%) of the samples from local markets and 27 (34%) from small butcher's shops were contaminated with Clostridium spp. Furthermore, C. perfringens was isolated from two (12%) and 15 (19%) samples from local markets and small butcher's shops, respectively. Mean counts of Clostridium spp. were 2.2 +/- 0.83 x 10(2) CFU g(-1) for local markets and 4.35 +/- 8.53 x 10(2) CFU g(-1) for small butcher's shops; mean counts for C. porringers were 2.75 +/- 0.21 x 10(2) and 6.82 +/- 10.96 x 10(2) CFU g(-1) from markets and butcher's shops, respectively. The number of samples contaminated with both Clostridium spp. and C. perfringens was higher in small butcher's shops than in local markets. Moreover, higher numbers of Clostridium spp. and C. perfringens were isolated in samples from small butcher's shops than from local markets. A total of 13 (13%) samples were also positive for toxins produced by the organism, as detected by ELISA. Eleven samples from small butcher's shops and two samples from local markets were positive for the C. perfringens toxins tested. Moreover, two (12%), one (1%), four (4%) and two (2%) samples were contaminated with C. perfringens types A, B, C and D, respectively. In conclusion, some meat samples collected from local markets and small butcher's shops contained C. perfringens and its toxins and, therefore, present a potential risk of food poisoning.

本研究的目的是确定产气荚膜梭菌及其毒素在肉糜中的流行程度。在土耳其卡尔斯的当地市场(16个)和小肉店(80个)共采集了96个肉末样本。使用市售ELISA试剂盒分析样品是否存在产气荚膜梭菌及其毒素。共分离到31株(32%)梭状芽孢杆菌,其中17株(55%)为产气荚膜梭状芽孢杆菌。当地市场4份(25%)和小型肉店27份(34%)样品中检出梭状芽孢杆菌,当地市场2份(12%)和小型肉店15份(19%)样品中检出产气荚膜杆菌。本地市场梭状芽孢杆菌平均计数为2.2 +/- 0.83 × 10(2) CFU g(-1),小型肉铺平均计数为4.35 +/- 8.53 × 10(2) CFU g(-1);来自市场和肉店的C. porringers平均计数分别为2.75 +/- 0.21 x 10(2)和6.82 +/- 10.96 x 10(2) CFU g(-1)。同时受梭状芽孢杆菌和产气荚膜梭菌污染的样本数目在小型肉店高于在本地市场。此外,小型肉店样品中分离出的梭状芽孢杆菌和产气荚膜梭菌数量高于当地市场样品。经ELISA检测,共有13份(13%)样本对该生物产生的毒素呈阳性。在小型肉店抽取的十一个样本及在本地街市抽取的两个样本对产气荚膜梭菌毒素测试呈阳性反应。A、B、C、D型产气荚膜梭菌分别有2份(12%)、1份(1%)、4份(4%)和2份(2%)。总之,从当地市场和小型肉店收集的一些肉类样本含有产气荚膜杆菌及其毒素,因此存在食物中毒的潜在风险。
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引用次数: 22
Allium cepa chromosome aberration and micronucleus tests applied to study genotoxicity of extracts from pesticide-treated vegetables and grapes. 大蒜染色体畸变及微核试验应用于农药处理蔬菜和葡萄提取物的遗传毒性研究。
Pub Date : 2007-06-01 DOI: 10.1080/02652030601113602
D Feretti, I Zerbini, C Zani, E Ceretti, M Moretti, S Monarca

The Allium cepa assay is an efficient test for chemical screening and in situ monitoring for genotoxicity of environmental contaminants. The test has been used widely to study genotoxicity of many pesticides revealing that these compounds can induce chromosomal aberrations in root meristems of A. cepa. Pesticide residues can be present in fruit and vegetables and represent a risk for human health. The mutagenic and carcinogenic action of herbicides, insecticides and fungicides on experimental animals is well known. Several studies have shown that chronic exposure to low levels of pesticides can cause birth defects and that prenatal exposure is associated with carcinogenicity. This study evaluated the potential application of plant genotoxicity tests for monitoring mutagens in edible vegetables. The presence of pesticides and genotoxic compounds extracted from 21 treated vegetables and eight types of grapes sampled from several markets in Campania, a region in Southern Italy, was monitored concurrently. The extracts were analysed for pesticides by gas chromatography and high-performance liquid chromatography, and for genotoxicity using two plant tests: the micronucleus test and the chromosomal aberration test in A. cepa roots. Thirty-three pesticides were detected, some of which are not approved. Genotoxicity was found in some of the vegetables and grapes tested. Allium cepa tests proved to be sensitive in monitoring genotoxicity in food extracts. The micronucleus test in interphase cells gave a much higher mutagenicity than the chromosomal aberration test in anaphase-telophase cells.

cepa试验是一种有效的化学筛选和环境污染物遗传毒性原位监测试验。该试验已被广泛应用于多种农药的遗传毒性研究,揭示了这些化合物可引起A. cepa根分生组织的染色体畸变。农药残留可能存在于水果和蔬菜中,对人体健康构成威胁。除草剂、杀虫剂和杀菌剂对实验动物的致突变和致癌作用是众所周知的。几项研究表明,长期接触低水平的农药会导致出生缺陷,产前接触与致癌性有关。本研究评价了植物遗传毒性试验在可食用蔬菜诱变剂监测中的潜在应用。同时监测了从意大利南部坎帕尼亚地区几个市场取样的21种处理过的蔬菜和8种葡萄中提取的农药和基因毒性化合物的存在。采用气相色谱法和高效液相色谱法对提取物进行了农药分析,并采用两种植物试验:微核试验和染色体畸变试验对菟丝子根进行了遗传毒性分析。共检出33种农药,其中部分农药未获批准。在一些接受测试的蔬菜和葡萄中发现了遗传毒性。事实证明,葱属植物对食品提取物的遗传毒性监测非常敏感。间期细胞微核试验的致突变性明显高于后期、末期细胞染色体畸变试验。
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引用次数: 70
Exposure assessment for fumonisins in the former Transkei region of South Africa. 南非前特兰斯凯地区伏马菌素暴露评估。
Pub Date : 2007-06-01 DOI: 10.1080/02652030601101136
G S Shephard, W F O Marasas, H-M Burger, N I M Somdyala, J P Rheeder, L Van der Westhuizen, P Gatyeni, D J Van Schalkwyk

The fumonisins are mycotoxins produced mainly by Fusarium verticillioides and F. proliferatum in maize, the predominant cereal staple for subsistence farming communities in southern Africa. In order to assess exposure to these mycotoxins in the Bizana (now known as Mbizana) and Centane magisterial areas of the former Transkei region of the Eastern Cape Province of South Africa, the actual maize consumption by different age groups in these communities was measured. In the groups 1-9 years (n = 215) and 10-17 (n = 240) years, mean consumption (+/-standard error) was 246 +/- 10.8 and 368 +/- 10.3 g per person day(-1), respectively, with no significant difference (p > 0.05) between the magisterial areas. For adults (18-65 years) mean maize consumption in Bizana (n = 229) and Centane (n = 178) were significantly different (p < 0.05) at 379 +/- 10.5 and 456 +/- 11.9 g per person day(-1), respectively. An exposure assessment was performed by combining the maize consumption distribution with previously determined levels of total fumonisin (fumonisins B(1) and B(2) combined) contamination in home-grown maize in these two areas. Assuming an individual adult body weight of 60 kg, fumonisin exposure in Bizana, an area of relatively low oesophageal cancer incidence, was 3.43 +/- 0.15 microg kg(-1) body weight day(-1), which was significantly lower (p < 0.05) than that in Centane (8.67 +/- 0.18 microg kg(-1) body weight day(-1)), an area of high oesophageal cancer incidence. Mean fumonisin exposures in all age groups in both Bizana and Centane were above the provisional maximum tolerable daily intake (PMTDI) of 2 microg kg(-1) body weight day(-1) set by the Joint FAO/WHO Expert Committee on Food Additives.

伏马菌素是一种真菌毒素,主要由玉米中的黄萎病镰刀菌和增殖性镰刀菌产生,而玉米是南部非洲自给农业社区的主要谷物。为了评估在南非东开普省前特兰斯凯地区的比扎那(现称为Mbizana)和Centane行政地区接触这些真菌毒素的情况,对这些社区不同年龄组的实际玉米消费量进行了测量。1 ~ 9岁组(n = 215)和10 ~ 17岁组(n = 240)人均日食用量(+/-标准误差)分别为246 +/- 10.8 g和368 +/- 10.3 g(-1),各辖区间差异无统计学意义(p > 0.05)。在成人(18-65岁)中,Bizana (n = 229)和Centane (n = 178)的平均玉米消费量分别为379 +/- 10.5 g和456 +/- 11.9 g /人天(-1),差异显著(p < 0.05)。通过将这两个地区的玉米消费分布与先前确定的伏马菌素总污染水平(伏马菌素B(1)和B(2)组合)相结合,进行了暴露评估。假设成人个体体重为60 kg,食管癌发病率相对较低的比扎那地区伏马菌素暴露量为3.43 +/- 0.15 μ kg(-1)体重日(-1),显著低于食管癌高发地区Centane的暴露量(8.67 +/- 0.18 μ kg(-1)体重日(-1)(p < 0.05)。比扎那和Centane地区所有年龄组的伏马菌素平均暴露量均高于粮农组织/世卫组织食品添加剂联合专家委员会规定的临时最大可耐受日摄入量(PMTDI) 2微克千克(-1)体重日(-1)。
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引用次数: 131
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