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Current incidence of N-nitrosodimethylamine in beers worldwide. 目前全球啤酒中n -亚硝基二甲胺的发病率。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701278354
E D Baxter, I R Slaiding, V Travers

A range of beers (n = 138) from 42 countries were analysed for the presence of N-nitrosodimethylamine (NDMA) using a chemiluminescence technique with a limit of quantification of 0.1 microg L(-1). The overwhelming majority of samples (79%) did not contain detectable NDMA, and only three samples exceeded 0.5 microg L(-1). No association was found between NDMA content and beer strength, type or geographical origin. It was noted that water can be a potential source of NDMA in beverages.

使用化学发光技术分析了来自42个国家的一系列啤酒(n = 138)中n -亚硝基二甲胺(NDMA)的存在,定量限为0.1 μ g L(-1)。绝大多数样品(79%)不含可检测的NDMA,只有三个样品超过0.5 μ g L(-1)。NDMA含量与啤酒度数、啤酒种类和产地没有关联。有人指出,水可能是饮料中NDMA的潜在来源。
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引用次数: 14
Changes in histamine and microbiological analyses in fresh and frozen tuna muscle during temperature abuse. 在温度滥用期间,新鲜和冷冻金枪鱼肌肉组胺和微生物分析的变化。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701278321
Vagelis Economou, Moira M Brett, Chrissanthy Papadopoulou, Stathis Frillingos, Tom Nichols

Temperature abuse of tuna (Thunnus alalunga) was carried out in order to assess the histamine buildup in fish-processing facilities where fish can be exposed to high temperatures for short periods of time. Histamine production was studied in tuna loins under different storage and abuse conditions. Tuna was stored at 0-2 degrees C, 3-4 degrees C, and 6-7 degrees C, and abused for 2 h daily at 20 degrees C and 30 degrees C for 7-12 days. Loins abused at 30 degrees C for 2 h daily contained potentially toxic histamine concentrations (67-382 mg kg(-1)) when stored at a low refrigeration temperature (0-2 degrees C), whereas when stored at 6-7 degrees C, the loins contained highly toxic histamine concentrations (544.5-4156.6 mg kg(-1)). Lower histamine concentrations (23-48 mg kg(-1) in loins stored at 0-2 degrees C and 124.7-2435.8 mg kg(-1) in loins stored at 6-7 degrees C) were observed in temperature-abused loins that were initially frozen. An increase over time was observed in most microbial counts tested. Bacteria isolated from the temperature-abused loins showed a varied ability of histamine production, with Morganella morganii, Klebsiella oxytoca, Staphylococcus hominis, and Enterococcus hirae being the most active histamine-producing bacteria.

对金枪鱼(Thunnus alalunga)进行温度滥用是为了评估鱼类加工设施中组胺的积累,在这些设施中,鱼类可以短时间暴露在高温下。研究了金枪鱼腰肉在不同贮藏和滥用条件下的组胺产量。金枪鱼分别储存在0-2℃、3-4℃和6-7℃,在20℃和30℃下每天虐待2小时,持续7-12天。在30℃下每天处理2小时的腰肉在低温(0-2℃)下储存时,其组胺浓度为67-382 mg kg(-1),而在6-7℃下储存时,其组胺浓度为544.5-4156.6 mg kg(-1))。在最初冷冻的温度虐待的腰肉中,组胺浓度较低(0-2℃储存的腰肉中组胺浓度为23-48 mg kg(-1), 6-7℃储存的腰肉中组胺浓度为124.7-2435.8 mg kg(-1))。随着时间的推移,大多数测试的微生物数量都有所增加。从受热腰肉中分离出的细菌显示出不同的组胺生产能力,其中莫氏摩根菌、氧化克雷伯菌、人型葡萄球菌和平氏肠球菌是最活跃的组胺生产细菌。
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引用次数: 40
Decline of pesticide residues from barley to malt. 从大麦到麦芽的农药残留减少。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701245189
S Navarro, G Pérez, G Navarro, N Vela

The fate of dinitroaniline herbicides (pendimethalin and trifluralin), organophosphous insecticides (fenitrothion and malathion), and pyrimidine (nuarimol) and triazole (myclobutanil and propiconazole) fungicides from barley to malt was determined. Several samples for residue analysis were taken after each stage of malting (steeping, germination and kilning). Pesticide residue analysis was carried out by GC/ITMS in selected ion monitoring mode. Pesticides decline along the process, although in different proportions. The carryover of residues after steeping was 45-85%. A good correlation (r > 0.92) was observed between percentages removed after steeping and the P(OW) values of pesticides. The amount remaining after malting ranged from 13 to 51% for fenitrothion and nuarimol, respectively. Steeping was the most important stage in the removal of pesticide residues (52%) followed by germination (25%), and kilning (drying and curing, 23%). During malt storage (3 months) the fall in pesticide residues was not significant. Applying the standard first-order kinetics equation (r > 0.95), the half-lives obtained for the pesticides during malt storage varied from 244 to 1533 days for myclobutanil and nuarimol, respectively.

测定了大麦和麦芽中二硝基苯胺类除草剂(戊二甲基灵和三氟灵)、有机磷类杀虫剂(非硝硫磷和马拉硫磷)、嘧啶类杀虫剂(nuarimol)和三唑类杀虫剂(myclobutanil和propiconazole)的去势。在每个阶段(浸泡、发芽和烧制)后取几个样品进行残留物分析。在选定的离子监测模式下,采用GC/ITMS进行农药残留分析。农药在这一过程中减少,尽管比例不同。浸泡后残留物的携带率为45-85%。浸泡后的去除率与农药的P(OW)值呈良好的相关(r > 0.92)。菲硝硫磷和nuarimol发酵后的残留量分别为13% ~ 51%。浸泡是去除农药残留最重要的阶段(52%),其次是发芽(25%)和烘烤(干燥和固化,23%)。贮藏期间(3个月)农药残留量下降不显著。应用标准一阶动力学方程(r > 0.95),在麦芽贮藏过程中,丁腈菌酯和nuarimol的半衰期分别为244 ~ 1533天。
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引用次数: 31
Occurrence of chloropropanols in soy sauce and other foods in China between 2002 and 2004. 2002 年至 2004 年中国酱油和其他食品中氯丙醇的含量。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701246039
Wu Sheng Fu, Yunfeng Zhao, Gong Zhang, Lei Zhang, Jing Guang Li, Chang Dong Tang, Hong Miao, Jin Bo Ma, Qi Zhang, Yong Ning Wu

A survey of chloropropanols in soy sauce and some selected foods in China is reported. Thirty-seven traditionally brewed soy sauce samples contained 3-MCPD below the EC maximum limit (ML) of 0.02 mg kg(-1). All soy sauce samples (629) from retailers contained levels of 3-MCPD ranging between <0.005 (LOQ) and 189 mg kg(-1), and only 12.2% had levels in excess of the Chinese ML of 1.0 mg kg(-1) for acid hydrolyzed vegetable protein (acid HVP). This indicates that the necessary processing changes have been made to decrease levels of chloropropanols in soy sauce. 2-Monochloropropane-1,3-diol (2-MCPD), 1,3-dichloro-2-propanol (1,3-DCP) and 2,3-dichloro-1-propanol (2,3-DCP) were detected in 48.1 19.1 and 3.78% of the soy sauce samples, respectively; the highest levels being 20.3, 8.26 and 0.50 mg kg(-1), respectively. A good linear correlation was found between the amount of 3-MCPD and 2-MCPD, with the level of 3-MCPD being generally higher than that of other chloropropanols for the same soy sauce. Acid HVP contained 3-MCPD at a level of 0.010-117.7 mg kg(-1) (on a liquid basis) and 80% of samples contained levels exceeding 1.0 mg kg(-1). In some other foods investigated, relatively high levels of 3-MCPD were found in soy sauce powder, oyster sauce, beef products, instant noodle spices and health foods, ranging from 0.029 to 13.64 mg kg(-1). It is concluded that abnormal levels of 3-MCPD in soy sauce or other foods produced in China may result from acid hydrolysis or the addition of the contaminated acid HVP.

报告对中国酱油和一些选定食品中的氯丙醇含量进行了调查。37 个传统酿造酱油样本的氯丙二醇含量低于 0.02 毫克/公斤(-1)的欧共体最高限量(ML)。所有来自零售商的酱油样本(629 个),氯丙二醇含量介乎 0.01 至 0.01 毫克/公斤(-1)之间。
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引用次数: 24
Study on the effect of grain storage and processing on deltamethrin residues in post-harvest treated wheat with regard to baby-food safety requirements. 粮食储存和加工对采后处理小麦中溴氰菊酯残留影响的婴儿食品安全要求研究
Pub Date : 2007-08-01 DOI: 10.1080/02652030701278313
Anna M Balinova, Rositsa I Mladenova, Deyana D Shtereva

The effects of storage intervals and of milling procedures on dissipation of deltamethrin residues in post-harvest treated wheat grain were studied with the aim to obtain scientific data on compliance of the processed products with the safety requirements concerning baby foods. The insecticide formulation was applied on stored wheat at a recommended rate of active ingredient of 0.5 mg kg(-1) and at a higher rate of 4 mg kg(-1), performing the highest protective effect. The dissipation of residues and their distribution in different fractions of the milled grain were studied after various storage intervals, from 7 to 270 days after treatment. Eight fractions - bran, semolina, three types of groats, and three types of flour - were collected after milling of grain and analysed for determination of pesticide residues. The residues were determined by gas chromatography characterized by the limit of determination of 0.005 mg kg(-1), low enough for enforcement of the maximum residue level of 0.01 mg kg(-1) established by the European Commission Directive for any pesticide in cereal-based foods. Deltamethrin applied post-harvest on wheat as grain protectant was distinguished by low rate of degradation on the grain under practical storage conditions. One hundred and eighty days after treatment at an application rate of 0.5 mg kg(-1), the residues were between 0.03 and 0.2 mg kg(-1) in the various types of flour. Two hundred and seventy days after treatment at a rate of 4 mg kg(-1), the residues in the flour were in the range of 0.4-1.5 mg kg(-1).

研究了采后处理小麦籽粒中溴氰菊酯残留的贮存间隔和碾磨工艺对其残留消散的影响,旨在获得加工产品是否符合婴儿食品安全要求的科学数据。该杀虫剂配方以有效成分推荐用量0.5 mg kg(-1)和更高用量4 mg kg(-1)施用于储存小麦,具有最高的保护效果。在处理后7 ~ 270 d的不同贮藏时间内,研究了残渣的耗散及其在不同颗粒中的分布情况。在谷物碾磨后,收集了麸皮、粗粒小麦粉、三种粗粒和三种面粉等八种馏分,并对其进行了分析,以测定农药残留。采用气相色谱法测定残留,测定限为0.005 mg kg(-1),足以执行欧盟委员会指令规定的谷物类食品中任何农药的最大残留限量0.01 mg kg(-1)。溴氰菊酯在小麦收获后作为谷粒保护剂,在实际贮藏条件下对谷粒降解率低。在施用量为0.5 mg kg(-1)的情况下,180天后,各类面粉的残留量在0.03 ~ 0.2 mg kg(-1)之间。以4 mg kg(-1)处理270 d后,面粉中的残留在0.4 ~ 1.5 mg kg(-1)之间。
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引用次数: 17
Methylmercury determination in fish and seafood products and estimated daily intake for the Spanish population. 鱼和海产品中甲基汞的测定及西班牙人口每日估计摄入量。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701258760
I Sahuquillo, M J Lagarda, M D Silvestre, R Farré

The mercury content of 25 samples of fish and seafood products most frequently consumed in Spain was determined. A simple method comprising cold vapour and atomic absorption spectrometry was used to determine separately inorganic and organic mercury. In all samples inorganic mercury content was below 50 microg kg(-1). There was wide variability, among not only the mercury levels of different fish species, but also for different samples of the same species - with the methylmercury content ranging from below 54 to 662 microg kg(-1). The highest mean methylmercury content was found in fresh tuna. Based on an average total fish consumption of 363 g/person week(-1), the methylmercury intake was estimated to be 46.2 microg/person week(-1). Therefore, the mercury intake of Spanish people with a body weight < or = 60 kg is lower than the Joint FAO/WHO Expert Committee on Food Additives (JECFA) provisional tolerable weekly intake (PTWI) of 1.6 microg kg(-1) body weight, but exceeds the US National Research Council (NRC) limit of 0.7 microg kg(-1) body weight week(-1) based on a benchmark dose.

对西班牙最常食用的25种鱼和海鲜产品样品的汞含量进行了测定。采用冷蒸汽原子吸收光谱法分别测定了无机汞和有机汞。所有样品的无机汞含量均低于50微克千克(-1)。不仅不同鱼种的汞含量存在很大差异,而且同一鱼种的不同样品也存在很大差异——甲基汞含量在54至662微克公斤(-1)以下。新鲜金枪鱼的甲基汞平均含量最高。根据鱼的平均总消费量为363克/人周(-1),甲基汞摄入量估计为46.2微克/人周(-1)。因此,体重<或= 60公斤的西班牙人的汞摄入量低于粮农组织/世卫组织食品添加剂联合专家委员会(JECFA)临时可耐受周摄入量(PTWI) 1.6微克千克(-1)体重,但超过了美国国家研究委员会(NRC)基于基准剂量的0.7微克千克(-1)体重周(-1)的限值。
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引用次数: 27
Improved microbial screening assay for the detection of quinolone residues in poultry and eggs. 禽蛋中喹诺酮类药物残留微生物筛选方法的改进。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701295275
M G Pikkemaat, P P J Mulder, J W A Elferink, A de Cocq, M W F Nielen, H J van Egmond

An improved microbiological screening assay is reported for the detection of quinolone residues in poultry muscle and eggs. The method was validated using fortified tissue samples and is the first microbial assay to effectively detect enrofloxacin, difloxacin, danofloxacin, as well as flumequine and oxolinic acid, at or below their EU maximum residue limits (MRL). The accuracy of the assay was shown by analysing incurred tissue samples containing residue levels around the MRL. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) quantification of the quinolone concentration in these samples showed that the test plate can be used semi-quantitatively, allowing the definition of an "action level" as an inhibition zone above which a sample can be considered "suspect". The presented assay is a useful improvement or addition to existing screening systems.

报道了一种改进的微生物筛选试验,用于检测家禽肌肉和鸡蛋中的喹诺酮类药物残留。该方法使用强化组织样本进行了验证,并且是第一个有效检测恩诺沙星、双氧沙星、达诺沙星以及氟喹和氧喹啉酸的微生物检测方法,达到或低于欧盟最大残留限量(MRL)。通过分析含有MRL周围残留水平的组织样本,证明了该测定法的准确性。液相色谱-串联质谱(LC-MS/MS)对这些样品中的喹诺酮浓度进行定量分析表明,该测试板可以半定量地使用,允许将“作用水平”定义为抑制带,超过该抑制带的样品可被视为“可疑”。所提出的分析是对现有筛选系统的有益改进或补充。
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引用次数: 38
Survey of pesticide residues in table grapes: determination of processing factors, intake and risk assessment. 鲜食葡萄中农药残留调查:加工因素测定、摄入量及风险评估。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701245320
M E Poulsen, H K Hansen, J J Sloth, H B Christensen, J H Andersen

The differences in residue pattern between Italy and South Africa, the main exporters of table grapes to the Danish market, were investigated. The results showed no major differences with respect to the number of samples with residues, with residues being found in 54-78% of the samples. Exceedances of the European Union maximum residue limit (MRL) were found in five samples from Italy. A number of samples were rinsed to study the possible reduction of residues. For copper, iprodione, procymidone and dithiocarbamates a significant effect of rinsing was found (20-49% reduction of residues). However, no significant effect was found for organophosphorus pesticides and pyrethroids, whereas the number of samples with residues of benzilates, phenylamids and triazoles was insufficient to demonstrate any significant effects. An intake calculation showed that the average intake from Italian grapes was 3.9 microg day(-1) for pesticides and 21 microg day(-1) for copper. Correspondingly, the intakes from South African grapes were 2.6 and 5.7 microg day(-1), respectively. When the total exposure of pesticides from grapes were related to acceptable daily intake, expressed as the sum of Hazard Quotients, the exposure were approximately 0.5% for Italian samples and 1% for South African samples.

研究了意大利和南非这两个向丹麦市场出口鲜食葡萄的主要国家在残留模式上的差异。结果显示,在含有残留物的样品数量方面没有重大差异,在54-78%的样品中发现了残留物。来自意大利的五个样品超过欧盟最大残留限量(MRL)。许多样品被冲洗,以研究可能减少残留物。对于铜、异丙二酮、原胺酮和二硫代氨基甲酸酯,发现冲洗效果显著(残留物减少20-49%)。然而,有机磷农药和拟除虫菊酯未发现显著影响,而苯甲酸酯类、苯胺类和三唑类残留的样本数量不足,不足以证明有任何显著影响。摄入量计算表明,意大利葡萄的平均农药摄入量为3.9微克/天(-1),铜摄入量为21微克/天(-1)。相应的,南非葡萄的摄入量分别为2.6和5.7微克天(-1)。当葡萄中农药的总暴露量与可接受的每日摄入量相关时,以危害商的总和表示,意大利样品的暴露量约为0.5%,南非样品的暴露量约为1%。
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引用次数: 37
Occurrence of tetrodotoxin and paralytic shellfish poisons in a gastropod implicated in food poisoning in southern Taiwan. 台湾南部发生与食物中毒有关的腹足动物的河豚毒素和麻痹性贝类中毒。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701245171
H-C Jen, S-J Lin, S-Y Lin, Y-W Huang, I-C Liao, O Arakawa, D-F Hwang

The toxicity of the gastropod Nassarius papillosus implicated in a food paralytic poisoning incident in Liuchiu Island, Taiwan, in October 2005 is reported. The symptoms of a victim (67 years old) were featured by general paresthesia, paralysis of phalanges and extremities, paralysis, coma, and aphasia. The remaining specimens of shell were assayed for toxicity. The range of specimen toxicity was found to be 63-474 mouse units (MU) per specimen for N. papillosus by a tetrodotoxin (TTX) bioassay. The mean (SD) toxicity of the digestive gland and other portions were 296 +/- 120 and 382 +/- 156 MU in N. papillosus. The toxin was partially purified from the acidic methanol extract of the gastropod by using a C18 solid-phase extraction column. The eluate was then filtered through a 3000 MW cut-off ultrafree microcentrifuge filter. It was shown that the toxin purified from gastropods analysed by high-performance liquid chromatography and liquid chromatography/mass spectrometry contained TTX 42-60 microg g(-1) (about 90%), whereas along with minor paralytic shellfish poisons (PSP) it was 3-6 microg g(-1) (about 10%).

报告2005年10月台湾柳球岛食物麻痹中毒事件中涉及的腹足动物乳头状腹足动物的毒性。1例患者(67岁)的症状为全身感觉异常、指骨和四肢麻痹、麻痹、昏迷和失语。对剩余的贝壳标本进行毒性测定。通过河豚毒素(TTX)生物测定,发现每个样本的毒性范围为63-474个小鼠单位(MU)。消化腺和其他部位的平均(SD)毒性分别为296 +/- 120 μ和382 +/- 156 μ。采用C18固相萃取柱从腹足动物的酸性甲醇提取物中部分纯化毒素。然后通过3000mw截止超自由微离心机过滤器过滤洗脱液。高效液相色谱和液相色谱/质谱分析表明,从腹足类中纯化的毒素含有TTX 42-60微克(-1)(约90%),而与轻微麻痹性贝类毒素(PSP)一起,其含量为3-6微克(-1)(约10%)。
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引用次数: 38
Validation of an ion-pair liquid chromatography-electrospray-tandem mass spectrometry method for the determination of heterocyclic aromatic amines in meat-based infant foods. 离子对液相色谱-电喷雾-串联质谱法测定婴儿肉类食品中杂环芳香胺的验证。
Pub Date : 2007-08-01 DOI: 10.1080/02652030701278339
F Calbiani, M Careri, L Elviri, A Mangia, I Zagnoni

A method based on ion-pair liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS) is reported for determining heterocyclic aromatic amines (HAAs) in meat-based infant foods. The HAAs encompassed quinoline (IQ, MeIQ), quinoxaline (MeIQx), pyridine (PhIP), and carboline derivatives (AalphaC, Harman, Norharman) with d(3)-IQ, (13)C(2)-MeIQx, and d(3)-PhIP used as labelled internal standards. The method used extraction into acetone followed by a clean-up on an SCX solid-phase extraction column. LC separation was performed on a TSKgel ODS-80TS column (250 x 2.0 mm, 5 microm), the mobile phase being an ammonium formate-formic acid buffer (3.03 mM ammonium formate, pH = 2.8) aqueous solution-acetonitrile gradient at a flow rate of 0.2 ml min(-1). For unequivocal identification of each analyte, three ions were detected and chosen for selected reaction monitoring (SRM). Validation was carried out on lyophilized meat samples. Mean recoveries ranged between 78 +/- 4% and 98 +/- 2% for different analytes. Limits of quantification generally lower than 8 ng g(-1) were demonstrated in meat samples for the analytes investigated. The method exhibited a good linearity and repeatability. Robustness testing identified those factors which were statistically significant in influencing chromatographic separation and response, and indicated which parameters have to be strictly controlled for a reliable analysis of HAAs. In particular, the mobile-phase flow rate was found to be statistically significant (alpha = 0.05) for the capacity factor (k') of all analytes except for AalphaC peak, whereas the mobile-phase pH resulted to be a critical parameter for the k' values of IQ, MeIQ, and Norharman. The method was proved to be robust vs. resolution between IQ and MeIQ peaks. Among mass-spectrometric parameters, collision energy was found to significantly affect quantitative response of all analytes except that of IQ. The applicability of the method to the analysis of meat-based infant food samples was demonstrated.

报道了一种基于离子对液相色谱-电喷雾串联质谱(LC-MS/MS)的测定肉类婴儿食品中杂环芳香胺(HAAs)的方法。HAAs包括喹啉(IQ, MeIQ),喹啉(MeIQx),吡啶(PhIP)和羰基衍生物(AalphaC, Harman, Norharman),其中d(3)-IQ, (13)C(2)-MeIQx和d(3)-PhIP作为标记内标。该方法采用提取丙酮,然后在SCX固相萃取柱上进行清理。色谱柱为TSKgel ODS-80TS (250 × 2.0 mm, 5微米),流动相为甲酸铵-甲酸缓冲液(3.03 mm甲酸铵,pH = 2.8)水溶液-乙腈梯度,流速为0.2 ml min(-1)。为了明确鉴定每种分析物,检测三个离子并选择用于选定的反应监测(SRM)。对冻干肉类样品进行了验证。不同分析物的平均回收率在78 +/- 4%和98 +/- 2%之间。定量限通常低于8 ng g(-1)在肉类样品中被证实为所调查的分析物。该方法具有良好的线性和重复性。鲁棒性检验确定了影响色谱分离和响应的有统计学意义的因素,并指出哪些参数必须严格控制才能可靠地分析HAAs。特别是,除AalphaC峰外,所有分析物的容量因子(k′)的流动相流速均具有统计学意义(α = 0.05),而流动相pH是IQ、MeIQ和Norharman的k′值的关键参数。结果表明,该方法具有较好的鲁棒性。在质谱参数中,除IQ外,碰撞能量对分析物的定量响应均有显著影响。验证了该方法对婴儿肉类食品样品分析的适用性。
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引用次数: 13
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