Fast extraction and dilution flow injection mass spectrometry method for quantitative chemical residue screening in food

A prototype multiresidue method based on fast extraction and dilution of samples followed by flow injection mass spectrometric analysis is proposed here for high-throughput chemical screening in complex matrices. The method was tested for sulfonylurea herbicides (triflusulfuron methyl, azimsulfuron, chlorimuron ethyl, sulfometuron methyl, chlorsulfuron, and flupyrsulfuron methyl), carbamate insecticides (oxamyl and methomyl), pyrimidine carboxylic acid herbicides (aminocyclopyrachlor and aminocyclopyrachlor methyl), and anthranilic diamide insecticides (chlorantraniliprole and cyantraniliprole). Lemon and pecan were used as representative high-water and low-water content matrices, respectively, and a sample extraction procedure was designed for each commodity type. Matrix-matched external standards were used for calibration, yielding linear responses with correlation coefficients (r) consistently >0.99. The limits of detection (LOD) were estimated to be between 0.01 and 0.03 mg/kg for all analytes, allowing execution of recovery tests with samples fortified at ≥0.05 mg/kg. Average analyte recoveries obtained during method validation for lemon and pecan ranged from 75 to 118% with standard deviations between 3 and 21%. Representative food processed fractions were also tested, that is, soybean oil and corn meal, yielding individual analyte average recoveries ranging from 62 to 114% with standard deviations between 4 and 18%. An intralaboratory blind test was also performed; the method excelled with 0 false positives and 0 false negatives in 240 residue measurements (20 samples × 12 analytes). The daily throughput of the fast extraction and dilution (FED) procedure is estimated at 72 samples/chemist, whereas the flow injection mass spectrometry (FI-MS) throughput could be as high as 4.3 sample injections/min, making very efficient use of mass spectrometers with negligible instrumental analysis time compared to the sample homogenization, preparation, and data processing steps.     

Total lipid extraction of homogenized and intact lean fish muscles using pressurized fluid extraction and batch extraction techniques

The reliability and efficiency of pressurized fluid extraction (PFE) technique for the extraction of total lipid content from cod and the effect of sample treatment on the extraction efficiency have been evaluated. The results were compared with two liquid-liquid extraction methods, traditional and modified methods according to Jensen. Optimum conditions were found to be with 2-propanol/n-hexane (65:35, v/v) as a first and n-hexane/diethyl ether (90:10, v/v) as a second solvent, 115 degrees C, and 10 min of static time. PFE extracts were cleaned up using the same procedure as in the methods according to Jensen. When total lipid yields obtained from homogenized cod muscle using PFE were compared yields obtained with original and modified Jensen methods, PFE gave significantly higher yields, approximately 10% higher (t test, P < 0.05). Infrared and NMR spectroscopy suggested that the additional material that inflates the gravimetric results is rather homogeneous and is primarily consists of phospholipid with headgroups of inositidic and/or glycosidic nature. The comparative study demonstrated that PFE is an alternative suitable technique to extract total lipid content from homogenized cod (lean fish) and herring (fat fish) muscle showing a precision comparable to that obtained with the traditional and modified Jensen methods. Despite the necessary cleanup step, PFE showed important advantages in the solvent consumption was cut by approximately 50% and automated extraction was possible.     

A rapid method for assessment of plant residue quality

A simple, reproducible and new method (modified dehydrogenase activity measurement after 72 h; DHA 72) was developed to assess plant residue quality for decomposition. The method resulted in similar assessments of residue quality than measurements of the C:N ratio, lignin:N ratio, and lignin and polyphenol concentration (PRQI). Among 25 plant residues tested, there was a large variation of DHA 72 as found in other well‐established methods. Based on cluster analysis, plant residues were grouped in four different classes; highly decomposable, moderately decomposable, slowly decomposable, and least decomposable. It is concluded that DHA 72 can very well be used to screen plant residues for residue quality judgment. The proposed method is very simple and easy to handle.     

Formulas for calculation of extraction volumes for commonly used pesticide residue extraction procedures

Formulas are presented for the calculation of extraction volume for pesticide residue procedures that use a single extraction with acetone, acetonitrile, or methanol, with or without prior dilution of these solvents with water. These formulas account for the volume change on mixing and for the volume contribution from the soluble sugars sucrose, glucose, and fructose. Results using these formulas are in agreement with the observed volumes of such mixtures within 0.3% throughout the following ranges, expressed as percent water in the mixtures: 15-38% for acetone, 4.8-59% for acetonitrile, and 9.3-33% for methanol.     

耦合浮珠-超声辅助溶剂萃取法用于微藻采收及油脂提取

为了优化微藻生物柴油生产工艺,开发高效低耗的微藻采收与油脂提取技术,该研究使用优化浮珠浮选工艺对小球藻进行采收,随后选取小球藻-表面层状聚合物浮珠聚集体进行破壁提油处理,并通过响应面优化破壁工艺,建立一种新型耦合浮珠-超声辅助溶剂萃取工艺。结果表明,在超声时间为13 min,正己烷：异丙醇体积比例为4,微藻质量浓度为13.6 g/L,超声功率为254 W时,油脂提取效率较高,为18.91%。相比传统气浮法与超声辅助溶剂萃取法,该法采收效率、细胞破壁效率和饱和脂肪酸含量都达到了较高水平,分别为98.36%、90.19%和37.03%。因此,耦合浮珠-超声辅助溶剂萃取工艺是一种有效提取小球藻细胞中油脂的工艺。研究结果为微藻生物柴油制备工艺的发展提供科学依据。     

Modified method for the analysis of free fatty acids in fish

The objective of this study was the development of a method for the quantification of free fatty acids (FFA) using less aggressive reactants against the handler and the environment than those used in the classic method of Lowry and Tinsley. The modified procedure is a variation of the Lowry and Tinsley method employing cyclohexane in place of benzene. The use of benzene is prohibited in certain work processes and laboratories, and the competent authority in each country is actively promoting research into harmless or less harmful products that could replace benzene. A comparison with the traditional AOCS titration method for oil analysis was performed. FFA content in mackerel frozen at -10 degrees C was measured according to the three methods over a 12 month period. The results showed similar values, and good correlations were obtained.     

A method for extraction of pentachlorophenol from plant tissues

Pentachlorophenol (PCP) was extracted from well homogenized and acidified plant samples with diethyl ether. Partial purification was carried out by the partition of PCP between ether extract and aqueous sodium hydroxide (5%), then between the acidified sodium hydroxide solution and benzene. The final purification of PCP was achieved by its good gas chromatographic separation during the quantitative determination. Techniques for optimizing the efficiency of the method were described in detail. The efficiency of the method was found to increase with the increase of the starting quantities of PCP, where it reached 89.2% for amounts greater than 400 ng. The loss of PCP due to its presence in the plant tissues was 29.3 and 21.6% for concentrations of PCP lower than 35.5 and higher than 46.2 ppb in the plant respectively. The overall recovery of PCP from plant tissues was found to be about 60% and 70% at the mentioned low and high concentrations in the plant.     

A simple method for quantitative determination of ATP in soil

A simple method to measure soil ATP by the luciferin-luciferase system is described. The ATP is extracted from the soil by vigorous shaking with a sulfuric acid-phosphate solution for 15 min. An aliquot of the soil suspension is neutralized with a Tris-EDTA solution and mixed with a special ATP releasing reagent (NRB). ATP is measured after a 10 s exposure to the NRB reagent, followed by addition of luciferin-luciferase and integration over 10 s in a Lumacounter M 2080. The ATP content in soils which had been stored at 5°C for 90 days and then incubated at 25°C for 5 days, ranged from 0.37 to 7.52 μg ATP g^?1 dry wt, with standard deviations less than 10%. There was a close (r = 0.96) linear relationship between ATP content and biomass C determinated by fumigation for this group of soils. The soil biomass contained 4.2–7.1 μg ATP mg^?1 biomass C. The ATP content of the biomass declined during storage at 5°C for 210 days.     

比较四种提取技术分析沉积物中滴滴涕同系物

Four techniques, Soxhlet extraction （SOX）, ultrasonic extraction （USE）, fluidized-bed extraction （FBE） and accelerated solvent extraction （ASE） with different solvents （methanol, hexane/acetone and acetonitrile） were used for the extraction of DDT analogues in sediments. Results revealed that the four extraction techniques had high recoveries （〉 86.0%） with low standard deviations （〈 12.0%） for most of DDT analogues, meaning that they could all successfully extract DDT analogues in sediments. Accelerated solvent extraction using methanol and hexane/acetone （1：1）, fluidized-bed extraction using hexane/acetone （1：1） and the ultrasonic extraction using hexane/acetone （1：1） were comparable or better than Soxhlet extraction using hexane/acetone （1：1）. Considering solvent- and time-consumption, level of automation, and environmental risk, accelerated solvent extraction with hexane/acetone （1：1） was better than the other extraction techniques.     

基于模糊判别成分分析法的高光谱作物信息提取与分类

东北地区是中国主要的玉米种植区,同时也是中国易发生干旱的地区,干旱常态化严重制约着该地区玉米生产的稳定发展。以辽宁省春玉米为研究对象,在明确春玉米不同发育期干旱变化特征的基础上,基于FY-3A、MODIS、春玉米发育期和土壤相对湿度观测等数据,建立春玉米干旱遥感监测指标集,构建各发育期不同土层深度的土壤相对湿度遥感监测模型,并以2000年为例开展了辽宁省春玉米干旱监测的应用研究,结果表明：1993-2012年辽宁省春玉米在各个发育期均有干旱发生,其中1999-2002年为干旱高发期,乳熟期干旱最为严重;多指数协同配合能提高遥感手段对土壤相对湿度的监测能力,其中陆表水分指数对土壤相对湿度监测能力较强,其次是水分指数;利用构建的春玉米各发育期土壤相对湿度遥感监测模型,监测2001-2004年部分发育期和土层深度的干旱状况,总体监测准确率为73.32%;实现了2000年辽宁省春玉米发育期干旱等级动态监测,所得监测结果与当年农业气象观测记录在发育阶段和空间上都有很好的一致性,遥感监测结果正确。因此,此项研究对于大范围准确跟踪监测春玉米干旱,以及提高春玉米生产的防灾减灾能力具有重要意义。     

淡水鱼的连续式鱼鳞去除方法

为研究连续式鱼鳞的去除方法,以鲢鱼、鳊鱼、鲤鱼为试验对象,提出了一种以弹簧为主要去鳞结构的去鳞刷,并以弹簧外径、去鳞刷转速与去鳞刷直径等为主要因素,通过自制去鳞试验台研究了其对淡水鱼去鳞率和鱼体损伤的影响,表明弹簧外径、去鳞刷直径对淡水鱼去鳞率有显著影响,对鱼体损伤感官评价得分影响不显著,去鳞刷转速对去鳞率和鱼体损伤感官评价得分均有极显著影响。不同种鱼,其各自适宜的弹簧外径、去鳞刷直径与去鳞刷直径有所不同。确定了白鲢去鳞时弹簧外径、去鳞刷转速、去鳞刷直径的最优参数组合,即弹簧外径21 mm、去鳞刷转速1 120 r/min、去鳞刷直径90 mm。该研究可为连续式去鱼鳞机的研制提供依据。     

Application of the porapak q column extraction method for tomato flavor volatile analysis

The Porapak Q column method (PQM) was compared to the method of simultaneous distillation extraction (SDE) under reduced pressure for extraction of the volatile compounds produced by tomato cv. Momotaro. The PQM was found to be effective at trapping and isolating many low and high boiling point volatile compounds and at producing the very desirable natural ripe tomato flavor of extracts. The SDE method was less effective in isolating the higher boiling point volatile compounds and caused deterioration of volatile compounds due to the heating process that takes place during extraction, resulting in an unpleasant boiled green tomato flavor of extracts. The advantages of using the PQM are its simplicity and its high efficiency in isolating many volatile compounds from nonvolatile materials at room temperature. A total of 367 volatile compounds were isolated by the PQM. Of these, hexanal, (Z)-3-hexenal, (E)-2-hexenal, 2- and 3-methylbutanol, and 2-phenylethanol were relatively more abundant than other compounds and (Z)-3-hexenal showed the highest relative amount.     

High-performance immunoaffinity chromatography for drug residue analysis

High-performance immunoaffinity chromatography (IAC) is a potentially strong analytical tool for measurement of drug residues in various matrixes. Although the use of Immunoaffinity separations is not new, the application to drug residue analysis is in its infancy. The present paper discusses the production and purification of antibody, the preparation of columns, the theoretical basis of the analytical separation and elution, and variations of the analytical approach.     

HPLC method for analysis of free amino acids in fish using o-phthaldialdehyde precolumn derivatization

Precolumn derivatization applying o-phthaldialdehyde (OPA) was used to analyze free lysine, histidine, and ornithine, precursors of the respective biogenic amines cadaverine, histamine, and putrescine, which are considered indicators of fish quality and safety. This method uses 75% methanol to eliminate the use of strong acids as the extraction solution. Each analysis took 35 min, was reproducible, and allowed separation of primary amino acids in fish samples. A binary solvent delivery system coupled with a fluorescence detector and an Ultrasphere ODS column were utilized for HPLC separation. Linearity of the calibration curves was very good (r(2) = 0.99) for the amino acids of interest. Minimum concentrations of detection were 40 pmol/mL for histidine and lysine and 70 pmol/mL for ornithine. Average recoveries were 72% for lysine, 93% for histidine, and 98% for ornithine. This method used solvent gradient elution to study the levels of these analytes in mahi-mahi, bigeye tuna, and flounder.