Objective To compare different sample digestion methods and establish an accurate method for the determination of the total aluminum in wheat samples by inductively coupled plasma optical emission spectrometry(ICP-OES). Methods National standard substance rice powder (GBW10045) and corn powder (GBW10012) were digested by 4 kinds of different sample digestion methods, including microwave digestion method (HNO3-H2O2 digestive system, HNO3-HF-H2O2digestive system, HNO3-HF-HCL digestive system) and ultra wave digestion method (HNO3-HF-H2O2digestive system). The aluminum content was determined by ICP-OES. The accuracy and reliability of these methods were verified by recovery tests. Results The determination result of aluminum content in the standard reference material by the ultra wave digestion method (HNO3-HF-H2O2digestive system) was within the standard reference range, but the results of the other 3 kinds of sample pretreatment methods were far below the reference range. The calibration curve showed good linearity in the range of 0.04~5.0 mg/L with correlation of 0.9999, the limit of quantitation was 2.0 mg/kg, the recovery rate was 91%~118%, and the relative standard deviation (RSD) ranged from 1.4% to 4.5%. Conclusion There may be aluminum which is encapsulated by silicon in wheat samples. The wheat samples can be digested completely under the ultra-wave digestion (HNO3-HF-H2O2system), and it's more accurate and can be used for the determination of total aluminum in wheat samples.

A method was established for the simultaneous determination of 3-chloropropanol esters (3-MCPDE) and glycidol esters (GE) in different types of oil and lipid food products by gas chromatography-mass spectrometry (GC-MS).Optimizations on extraction,transesterification,derivatization and the chromatographic conditions of GC-MS of samples were completed.Limits of quantitation (LOQs) of the method for four types of food products,i.e.vegetable oils,milk powder,fried and puffed foods and bakery foods,were 100,25,125,20 μg/kg,respectively,the total mean recoveries were in the range of 81.2％-109％ with the relative standard deviations (RSD,n =6) of 0.77％-7.3％ and the correlation coefficients(r) higher than 0.999.Moreover,the 3-MCPDE and GE contents in 30 oil and lipid food products were determined to be in the range of no detected-8.04 mg/kg.The developed method could meet the demand for routine food inspection,in particular for the quantitative and qualitative determination of 3-MCPDE and GE in oil and lipid foods with its high efficiency,high sensitivity and strong workability.

To develop a isotope-labeled internal standard liquid chromatography tandem mass spectrometry(LC-MS/MS)method for the determination of vitamin D3 in foods for infants and young children.The sample was inoculated with a isotope-labeled internal standard and saponified with ethanol-50 ％ potassium hydroxide,followed by extraction with petroleum ether.The chromatographic separation was performed on the Adantis T3 column (100 mm× 2.1 mm,3 μm),using methanol-5 mmoL/L ammonium formate solution as the mobile phase by gradient elution.The method applied positive electrospray ionization and multiple reaction monitoring mode and quantified with peak area with internal standard method.A good linearity was obtained for 2～2000 μg/L with a correlation coefficient above 0.99.The average recoveries from three different were with the range of 86.1％ to 107％ and 86.2％ to 106％ respectively in formula and rice flour at spiked levels of 10,50,100 μg/kg.and the relative standard deviations were between 4.48 ％ to 7.08 ％ and 2.60 ％.to 4.26 ％ respectively(n=6).The limit of quantification was 10 μg/kg.This method is simple,accurate and suitable for determination of vitamin D3 in foods for infants and young children.

Mycotoxins not only contaminate food,but also cause serious harm to human health.The paper collected some relevant regulations on mycotoxins limit standards,which were published by contries as United States,Canada,Australia,New Zealand,Japan,Korea,regions as Hong Kong,Macao,Taiwan,and national organization as Codex Alimentarius Commission,European Union.Above all,a comprehensive comparison among the regulations was given to provide useful reference for promoting relevant standards to integrate with the intemational regulations,and thus improving the management and control of mycotoxins in food in the mainland of China.

目的 探讨石墨管性能变化对质控样南瓜粉中铅含量测定的影响,同时对铅标准溶液和样品消解液有效存放期进行研究.方法 采用石墨炉原子吸收光谱法和质量控制图法测定不同使用次数的石墨管下及不同存放时间的铅标准溶液下质控样中铅的含量.结果 在石墨管使用次数约1800次时,质控样绿茶(GBW10052(GSB-30))中的铅含量为1.38 mg/kg,达到质控图的警戒下限.1000 mg/L铅标准储备液在室温或4℃密封冷藏时,至少10个月内可进行质控样中铅的测定,样品消解液聚四氟乙烯瓶密封保存至少1个月内可进行质控样中铅的有效测定.结论 用质控样绘制质控图的方法可有效监测石墨管有效使用次数,当质控样铅检测结果接近警戒限时需要更换石墨管.本方法设计合理,操作简便,能有效保证食品中铅含量测试的准确和可靠性.

目的 建立超高效合相色谱测定植物油中丁基羟基茴香醚(BHA)和二丁基羟基甲苯(BHT)的方法.方法 样品以正庚烷-异丙醇提取,体积比为80:20;应用超高效合相色谱仪,采用超临界CO2和甲醇-乙腈(体积比为50:50)梯度洗脱,经ACQUITY UPC2 BEH 2-EP色谱柱分离,二极管阵列检测器检测,以保留时间定性,外标法峰面积定量.结果 样品在50～200 mg/kg范围内,BHA的平均回收率在96.1％～99.3％之间,相对标准偏差为1.11％～1.30％;BHT的平均回收率在93.8％～99.4％之间,相对标准偏差为0.5％～4.0％.BHA和BHT的定量限均为25 mg/kg.结论 该方法具有分析时间快、溶剂消耗少的优点,能快速分析植物油中的BHA和BHT.

建立了直接溶解-石墨炉原子吸收光谱法测定食品营养强化剂葡萄糖酸铜中重金属铅含量的方法.对样品前处理方法及测试方法进行了研究.结果表明,葡萄糖酸铜样品不宜进行常规的酸消化前处理,采用该方法对样品进行处理后,消解液有大量蓝色不溶物;本标准采用水直接溶解法.USP 36采用的标准加入法操作繁琐,需要多次手动稀释,增加了方法的测量不确定度.本方法采用标准曲线法进行铅含量的测定,用10g/L磷酸二氢铵和0.6g/L硝酸镁混合液作为基体改进剂,提高了灰化及原子化温度,该方法具有满意的准确度及精密度.在4.0 ～ 60ng/mL的线性范围内,线性方程为y=0.00259x+0.00128,线性相关系数为0.9990.回收率为85.8％ ～ 90.6％,相对标准偏差为4.2％～7.6％(n=8),检出限与定量限分别为0.23ng/mL和0.76ng/mL.该方法准确、可靠,适合于食品营养强化剂葡萄糖酸铜中重金属铅含量的测定.

To develop a ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the determination of 13 plant growth regulator residues in fruits and vegetables. The sample was extracted with methanol–H2O and the chromatographic separation was performed on the Shim-pack XR C18 column(75 mm × 2.0 mm,1.6 μm),using acetonitrile-0.1% acetic acid as the mobile phase by gradient elution. The method applied electrospray ionization in positive and negative multiple reaction monitoring mode and quantified with peak area with matrix-matched external standard method. A good linearity of Chlormequat chloride,Paclobutrazol,Uniconazole,thidiazuron,gibberellic acid 2-naphthaleneacetic acid,Forchlorfenuron,2,4-D,Cloprop,4-Chloroph-enoxyacetic acid,2,4,5-Trichlorophenoxyacetic acid,6-Benzylaminopurine and isopropyl N-(3-chlorophenyl)carbamate were in the concentration range of 1.0-20 μg/L with a correlation coefficient above 0.99. The average recoveries from three different were with the range of 81.2% to 106% at spiked levels of 10,20,50 μg/kg,and the relative standard deviations were between 2.13% to 11.8%(n=6). The limit of quantification was in the range of 0.022~16 μg/kg. This method is simple,selectivity and suitable for determination of 13 residues in fruits and vegetables.

To survey the application situation of plant growth regulators in fruits and vegetables, samples from local market, import and export of Guangzhou city, Shantou city, Zhongshan city and Huizhou city of Guangdong province were randomly collected. 445 samples of fruits and vegetables were collected to determine the residues of 13 kinds of plant growth regulators by ultra performance liquid chromatography mass spectrometry. The results showed that plant growth regulators detection rate was 55.5% and 24.3% in 330 local market samples and 115 import and export samples, respectively. Plant growth regulator CCC had the highest detection rate, products like grapes, tomato,cucumber had the highest detection rate.

To develop a liquid chromatography tandem mass spectrometry(LC-MS/MS)method for the determination of vitamin D3 in milk products.The sample was saponified with ethanol – 50 % potassium hydroxide,followed by extraction with hexane and cleaned up by saturated sodium chloride solution. The chromatographic separation was performed on the YMC C18 column(50 mm×2.1 mm,3μm),using methanol-5 mmol/L ammonium formate solution as the mobile phase by gradient elution. The method applied positive electrospray ionization and multiple reaction monitoring mode and quantified with peak area with internal standard method.A good linearity was obtained for 0-50μg/L with a correlation coefficient above 0.99.The average recoveries from three different were with the range of 83.9% to93.0% at spiked levels of 20,100,200μg/kg,and the relative standard deviations were between 1.10% to 4.90%(n=6).The limit of quantification was 20μg/kg. This method is simple, accurate and suitable for determination of vitamin D3 in milk products.

In this paper,the Maximum Residue Limit(MRLs) of plant growth regulator at home was summarized,and MRLs among China,CAC,EU,America and Australia was compared in order to provide the reference for the study and setting MRLs in plant growth regulator.There were significant gaps between China and abroad.Firstly,national MRLs in plant growth regulator was missing,and less than the number of actually approved species by country.Secondly,product categories and limits prescribed by national MRLs could not meet the requirements of importer of agricultural products.Thirdly,national MRLs in plant growth regulator focused on products of plant origin,did not include products of animal origin.At last,we put forward the following suggestions: as soon as possible to establish and perfect national MRLs in plant growth regulator that has approved,and considering setting MRLs in plant growth regulator in products of animal origin.

婴幼儿配方奶粉中添加有必需成分和可选择性成分等,针对这些添加成分的名称和来源,国家都有相关标准规定.该项调查对象是广州市售的来自国内外不同产地的58种婴幼儿配方奶粉外包装信息,分析其配料表中标注的可选择性成分(包括部分营养强化剂、菌种和食品添加剂),并与国家规定相比较.结果发现大部分产品都添加有牛磺酸、二十二碳六烯酸、花生四烯酸、低聚半乳糖、低聚果糖和核苷酸,而菌种、L-氨基酸等较少被添加.多数的添加成分符合我国相关规定,但也有少数标注不规范的情况.该研究还有助于消费者和相关专业人士深入了解婴幼儿配方奶粉的配料表.

目的 建立利用离子色谱/电导检测法同时测定食品中多种食品添加剂和非法添加物的分析方法.方法 不同样品经纯水稀释或提取后,样品溶液经固相萃取C18柱净化,经0.45 μm滤膜过滤后直接进样检测;选用lonpac AS11-HC阴离子交换分离柱,氢氧化钾淋洗液梯度洗脱,流速1.3 ml/min,以抑制电导检测器检测,外标法峰面积定量.结果 该方法对8种食品添加剂和2种非法添加物具有良好的线性,线性范围在0.05 mg/L～ 20 mg/L、0.1 mg/L ～20 mg/L,相关系数在0.9950 ～0.9998之间;准确度和精密度良好,样品加标回收率在73％ ～ 104％之间,RSD＜7.0％;定量限为2.5 mg/kg ～ 5.0 mg/kg.结论 该方法线性范围广,准确性和精密度良好,操作较简便,结果满意,能满足日常检验要求.

建立了婴幼儿配方奶粉中肌醇的液相色谱串联质谱法.样品经水溶液提取,用三氯甲烷沉淀蛋白后,用液相色谱串联质谱仪(C18柱)分析,流动相为0.2％乙酸∶甲醇(98∶2;体积比),流速为0.20 mL/min,柱温为40℃,肌醇以保留时间和多反应监测离子对定性,以内标法峰面积定量.乳粉样品中肌醇的回收率是94.7％～106％,RSD为1.80％～3.73％,线性范围在0.1～2.0 mg/kg,检出限为0.1 mg/kg.该方法操作简便、快速、准确,适用于乳粉中肌醇含量的测定.

The olive tree (Olea europaea), native to the coastal areas of eastern mediterranean basin and parts of Asia, nowadays is cultivated all around the world. The products of olive trees, including olive leaves, fruit and oil, possess high nutritional and medicinal values. The characteristic bioactivities of olive products include antioxidant, anti-cancer, anti-hypertension and anti-atherosclerosis and so on. The studies suggest that these benefits mainly come from its balance of polyunsaturate fatty acids and saturate fatty acids, together with the considerable amount of phenolics, sterols, tocopherols, etc. The objective of this review is to summarize the chemical components and bioactivities of Olea europaea.

A dispersive solid phase extraction-high performance liquid chromatographic (HPLC) method was established for the simultaneous determination of 2,4-D, thiabendazole, 2-naphthol, o-phenyl phenol, diphenyl ether and biphenyl in the fruits and vegetables. The samples were vortexed for extraction with acetonitrile containing sodium chloride and anhydrous magnesium sulfate. The acetonitrile extraction was purified by acidic alumina dispersed solid phase extraction. The analysis was performed on an Agilent TC C18 column (250 mm x 4.6 mm, 5 microm) and an ultraviolet detector at 235 nm with a mobile phase of methanol-0.02 mol/L (pH 6) potassium dihydrogen phosphate solution, at a flow rate of 1.0 mL/min with gradient elution. Good linearities were observed in the range of 0.5-20 mg/L with correlation coefficients greater than 0.99. The average recoveries of the six preservatives in fruits and vegetables were in the range of 84.2% -99. 1% at three spiked levels of 1, 2 and 10 mg/kg (n = 6) and the relative standard deviations (RSDs) were in the range of 1.67%-10.3%. The limits of quantification were 1 mg/kg. This method is simple, accurate and suitable for the determination of the six preservatives in fruits and vegetables.

2011年4月20日发布的GB 2760-2011标准，是在GB 2760-2007标准的基础上进行修订的。本次修订是以风险评估原则为基础，运用国际通用的食品添加剂风险评估原则、程序和方法，利用我国居民营养调查获得的居民食物摄入量数据和全国污染物监测网络获得的食品添加剂的监测数据，对安全性和食品工艺使用的必要性原则进行审查。

To develop a high performance liquid chromatographic(HPLC) method for the determination of benzoic acid and sorbic acid in soy, sauce and sauce product. Sample was extracted with acetonitrile after acidification by HCl-NaCl intermixture. The extractive was analyzed by C 18 column with ratio ammonium acetate(0.02 mol/L) and methanol of 95:5(v/v) at a flow rate of 1.0 mL/min, detected by PDA detector with 230 nm. Benzoic acid and sorbic acid was affi rmed according to retention time, and quantifi ed by peak area with external standard method. The recoveries of the method spiked at 4 levels(10 mg/kg, 20 mg/kg, 50 mg/kg and 100 mg/kg) were within the range of 91.5%~104%(benzoic acid) and 85.4%~100%(sorbic acid), with RSDs ranging from 1.11%~2.39%(benzoic acid) and 1.79%~4.09%(sorbic acid). The detection limit of the method was 10 mg/kg. The method is simple, accurate and suitable for the determination of benzoic acid and sorbic acid in soy, sauce and sauce product.

This paper is the translation of the European standard EN 13804:2013: Foodstuffs - Determina-tion of elements and their chemical species - General considerations and specific requirements. This standard specified the general considerations and special requirements for the determination of elements and their chemical species in food, including a process from receiving samples by the laboratory to the final test result. It mainly included the considerations and specific requirements such as reagents, apparatus, equipment and sto-rage requirements in the sample preparation and such as reagent, standard substance, containers and equipment in the analysis of trace elements in food, included the calculation method of the detection limit, quantitative limit, recovery rate and the measurement uncertainty,etc., included the quality assurance methods such as pro-ficiency testing schemes(PT), using standard material (RM) or certified standard material (CRM). It also in-cluded the expression of the test result and the essential content in a test report.