[Objectives]A rapid screening and analysis method for 26 organophosphorus agrochemicals in fresh milk was established using ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrome...[Objectives]A rapid screening and analysis method for 26 organophosphorus agrochemicals in fresh milk was established using ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry.[Methods]Raw milk was extracted with acetonitrile solution containing 0.2%formic acid by volume,and purified with a Dikma ProElut QuECHERS solid phase extraction cartridge.Target compounds were separated on a Waters ACQUITY UPLC HSS T3 chromatographic column(2.1 mm×50 mm,1.8μm)with methanol-water solution as a mobile phase for gradient elution,and through scanning with an electrospray ion source in positive ion mode,26 kinds of organophosphorus agrochemicals could be accurately qualitatively determined within 10 min.[Results]When using formic acid acetonitrile with a volume fraction of 0.2%,there were more types of detected compounds and a greater recovery;and using B cartridge could effectively eliminate the interference of non-polar substances such as phospholipids,achieve higher number of detected compounds than those of A and C,and well separate the 26 kinds of agrochemical residues.[Conclusions]This study provides a reference method for the rapid screening of agrochemical residues in dairy cows in the future.展开更多
The basic goal of this research was to determine the impact of the presence of bacterial (CFU) and somatic cells count content (SCC) in quality of fresh milk in some small cattle farms in Kosovo. The survey was based ...The basic goal of this research was to determine the impact of the presence of bacterial (CFU) and somatic cells count content (SCC) in quality of fresh milk in some small cattle farms in Kosovo. The survey was based on existing standards for milk quality in Kosovo placed under administrative guidance MA-no. 20/2006. The study was based on fresh milk analysis of 150 farms performed during the period September-December 2012, which was obtained in 9 different localities (collection points) of the Kosovo. Our study reveals that CFU and SCC in fresh milk were significantly affected by a number of factors, as: sampling period (repetition), locality, breed, and time of sampling (evening or/and morning). According to the results for CFU and SCC, there were big differences between the farms (milk collection points) included in the study (P < 0.0403) and (P < 0.0293). The results show that small size breed like Busha and its crosses tend to be less exposed to SCC/mL in milk (72.840) and (293.592), compared to Black Holstein (613.462), Simmental (521.519) and Brown Swiss (418.44). Milk produced in evening tended to be of better quality (259.854 CFU/mL) compared to the one from morning milking (576.689 CFU/mL). Fresh milk quality analyzed in the third repetition was better for about 33.3% compared with the repletion first. For CFU and SCC, the analyses show that about 74.7% and 64.7% of milk produced belongs to extra quality, while lower quality of milk of category three is 12.0% and 23.3%, respectively. Considering that about 85% of milk produced in Kosovo comes from small-scale dairy farms, the current study sets out that small-scale milk production system cannot be neglected by interest parties in dairy sector and needs permanent following up and improvement.展开更多
The moisturizing effect of a fresh-milk cream after single and long-term application was studied by the combination of subjective and instrumental methods.The purpose of this study was to evaluate the moisturizing eff...The moisturizing effect of a fresh-milk cream after single and long-term application was studied by the combination of subjective and instrumental methods.The purpose of this study was to evaluate the moisturizing efficacy of fresh milk as a moisturizer in skin care products.Thirty female subjects aged 18~55 years were enrolled and a randomized,double-blind,placebo-controlled comparison study was applied in this research.The stratum corneum water content and transdermal water loss on the cheek,and VISIA-CR images of the whole face were recorded after using the samples.The subjective evaluation of the subjects were also collected.The results showed that the fresh milk cream played a significant role in increasing the water content of facial stratum corneum,improving the transdermal water loss and skin redness compared with the base formula without fresh milk.It indicated that fresh milk can be added to skin care products as a moisturizing agent,which can replenish moisture and enhance the skin barrier function.展开更多
The reducing efficiencies of the commonly used heat treatment methods and fermentation processes on aflatoxin M1 (AFM1) in Nigeria were investigated. Seventy samples of fresh cow milk from both conventional and tradit...The reducing efficiencies of the commonly used heat treatment methods and fermentation processes on aflatoxin M1 (AFM1) in Nigeria were investigated. Seventy samples of fresh cow milk from both conventional and traditional dairy cattle herds were collected and analyzed for the determination of AFM1 using Cobra-cell incorporated high performance liquid chromatography. Of these analyzed samples, 56 (80.0%) tested positive for AFM1 out of which 3 milk samples with high AFM1 concentrations were selectively pooled and subjected to varied conditions of heat treatments and fermentation processes using both indigenized and exotic strains of lactic acid bacteria (Lactobacillus bulgaricus + Streptococcus thermophilus and L. rhamnosus and L. plantarum) as starter cultures respectively. Both processes used either singly or combined, demonstrated high degrees of reducing effects on AFM1 levels. Sterilization of the milk at 121?C and 80?C under the same condition of time (15 - 20) min showed significant reduction of up to 58.8% (p 0.05) in the level of AFM1 when compared with the initial mean AFM1 concentration of the untreated fresh milk. The situation was however different around the boiling temperature of 100?C at which point the level of AFM1 reduction was found to be inconsistent. The indigenized combined strains showed some slight margins of AFM1 reduction in the proportions of (20.5, 30.8 and 43.9)% over and above that of the exotic strains (17.4, 30.0 and 41.1)% in 12 h, 48 h and 72 h of fermentation respectively. Generally, fermentation alone showed lower reduction of AFM1 in milk from 24.5% to 43.9% compared with the reducing activities of (35.4 to 58.8)% when heat-treated milk samples were subsequently subjected to varied fermentation conditions.展开更多
A simple, accurate and sensitive high-performance liquid chromatography （HPLC） method was developed, validated and applied to the determination of either theophylline or paracetamol in milk-based samples. The method...A simple, accurate and sensitive high-performance liquid chromatography （HPLC） method was developed, validated and applied to the determination of either theophylline or paracetamol in milk-based samples. The method allowed drug quantification in fresh and powdered milk with a relatively short run time of analysis and it was also successfully applied to the quantification of the drugs in solid dosage forms intended for pediatric use. Moreover, the main significant advantages over other published works are the simplicity of the sample preparation, reduced assay time and sample loss. The method meets the International Conference on Harmonization guideline for analytical methods validation regarding specificity, linearity, accuracy, precision, specificity and robustness as required by health authorities and applied by industry while designing and marketing new drug products. The technique encompasses the separation of the analytes with a reverse phase C18 column under isocrafic conditions and UV detection at 272 nm and 243 nm, respectively, for theophylline and paraeetamol. The lower limit of quantification for both drugs was determined as 0.2 μg/mL and the between-batch accuracy was 99.7%. This HPLC method allows quantification of theophylline and paracetamol in milk matrices and it can be applied in the design, development and production of milk-based pediatric dosage forms.展开更多
The main objective of this study was to analyze the effect of bacterial content (CFU) and somatic cell count (SCC) in milk quality in sheep (Ovis aries) farms according to the existing standards for fresh milk quality...The main objective of this study was to analyze the effect of bacterial content (CFU) and somatic cell count (SCC) in milk quality in sheep (Ovis aries) farms according to the existing standards for fresh milk quality in Kosovo. A total of 2256 milk test day records from 379 Bardhoka (BAR), Sharri sheep (SHA), Kosovo sheep (KOS) and Balusha (BAL) ewes in eight herds across the country were collected and analyzed through a period April-October 2010. The general linear model and Duncan’s test were used to analyze the effect of different variables on presence of CFU and SCC in fresh milk. The effect of all variables was considered as a fixed. The overall results show that farm (P 0422), respectively, had a significant effect on presence of SCC. For CFU farm (P 0422) and breed (P 1211.17 to 6425.76 CFU/mL and 846.07 to 2043.15 SCC/mL milk, respectively. Although the rate of fresh milk contamination with SCC tends to be relatively low compare with CFU, by all means both variables should not be underestimated bearing in mind that a high rate of them on fresh milk are negatively correlated with farmer’s profit, consumer food safety and overall animal health.展开更多
In order to establish an HPLC-MS/MS method for detecting progesterone in raw milk,raw milk was extracted with methanol,and then determined by HPLC-MS/MS after the purification with a C18 solid phase extraction column....In order to establish an HPLC-MS/MS method for detecting progesterone in raw milk,raw milk was extracted with methanol,and then determined by HPLC-MS/MS after the purification with a C18 solid phase extraction column. Qualitative determination was performed according to retention time and selective ion abundance ratio,and quantification was performed by external standard method. The results showed that progesterone had a good linear relation in the range of0. 1-5. 0 ng/ml,with a correlation coefficient of 0. 999 9. The detection limit of the established method was 0. 02 μg/kg,and the quantification limit was0. 04 μg/kg. In the standard addition range of 0. 1-5. 0 ng/ml,the recovery ranged from 79. 6% to 105. 1%,with relative standard deviation≤8. 9%. Compared with the industry standard,the detection limit and the quantification limit of the established method are significantly reduced,and the sensitivity of the method is enhanced,so this method is suitable for the detection of progesterone residue in fresh milk in pastures.展开更多
基金Hebei Provincial Key R&D Project(19227516D)Hebei Provincial Phase II Modern Agricultural Industry Technology System Innovation Team Building Project(HBCT2018120207,HBCT2018160403).
文摘[Objectives]A rapid screening and analysis method for 26 organophosphorus agrochemicals in fresh milk was established using ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry.[Methods]Raw milk was extracted with acetonitrile solution containing 0.2%formic acid by volume,and purified with a Dikma ProElut QuECHERS solid phase extraction cartridge.Target compounds were separated on a Waters ACQUITY UPLC HSS T3 chromatographic column(2.1 mm×50 mm,1.8μm)with methanol-water solution as a mobile phase for gradient elution,and through scanning with an electrospray ion source in positive ion mode,26 kinds of organophosphorus agrochemicals could be accurately qualitatively determined within 10 min.[Results]When using formic acid acetonitrile with a volume fraction of 0.2%,there were more types of detected compounds and a greater recovery;and using B cartridge could effectively eliminate the interference of non-polar substances such as phospholipids,achieve higher number of detected compounds than those of A and C,and well separate the 26 kinds of agrochemical residues.[Conclusions]This study provides a reference method for the rapid screening of agrochemical residues in dairy cows in the future.
基金the support for the Ministry of Education Science and Technology of Republic of Kos-ovo for granting the study through the small grant project“Study of Autochthon Busha Cattle in Kosovo”.
文摘The basic goal of this research was to determine the impact of the presence of bacterial (CFU) and somatic cells count content (SCC) in quality of fresh milk in some small cattle farms in Kosovo. The survey was based on existing standards for milk quality in Kosovo placed under administrative guidance MA-no. 20/2006. The study was based on fresh milk analysis of 150 farms performed during the period September-December 2012, which was obtained in 9 different localities (collection points) of the Kosovo. Our study reveals that CFU and SCC in fresh milk were significantly affected by a number of factors, as: sampling period (repetition), locality, breed, and time of sampling (evening or/and morning). According to the results for CFU and SCC, there were big differences between the farms (milk collection points) included in the study (P < 0.0403) and (P < 0.0293). The results show that small size breed like Busha and its crosses tend to be less exposed to SCC/mL in milk (72.840) and (293.592), compared to Black Holstein (613.462), Simmental (521.519) and Brown Swiss (418.44). Milk produced in evening tended to be of better quality (259.854 CFU/mL) compared to the one from morning milking (576.689 CFU/mL). Fresh milk quality analyzed in the third repetition was better for about 33.3% compared with the repletion first. For CFU and SCC, the analyses show that about 74.7% and 64.7% of milk produced belongs to extra quality, while lower quality of milk of category three is 12.0% and 23.3%, respectively. Considering that about 85% of milk produced in Kosovo comes from small-scale dairy farms, the current study sets out that small-scale milk production system cannot be neglected by interest parties in dairy sector and needs permanent following up and improvement.
文摘The moisturizing effect of a fresh-milk cream after single and long-term application was studied by the combination of subjective and instrumental methods.The purpose of this study was to evaluate the moisturizing efficacy of fresh milk as a moisturizer in skin care products.Thirty female subjects aged 18~55 years were enrolled and a randomized,double-blind,placebo-controlled comparison study was applied in this research.The stratum corneum water content and transdermal water loss on the cheek,and VISIA-CR images of the whole face were recorded after using the samples.The subjective evaluation of the subjects were also collected.The results showed that the fresh milk cream played a significant role in increasing the water content of facial stratum corneum,improving the transdermal water loss and skin redness compared with the base formula without fresh milk.It indicated that fresh milk can be added to skin care products as a moisturizing agent,which can replenish moisture and enhance the skin barrier function.
文摘The reducing efficiencies of the commonly used heat treatment methods and fermentation processes on aflatoxin M1 (AFM1) in Nigeria were investigated. Seventy samples of fresh cow milk from both conventional and traditional dairy cattle herds were collected and analyzed for the determination of AFM1 using Cobra-cell incorporated high performance liquid chromatography. Of these analyzed samples, 56 (80.0%) tested positive for AFM1 out of which 3 milk samples with high AFM1 concentrations were selectively pooled and subjected to varied conditions of heat treatments and fermentation processes using both indigenized and exotic strains of lactic acid bacteria (Lactobacillus bulgaricus + Streptococcus thermophilus and L. rhamnosus and L. plantarum) as starter cultures respectively. Both processes used either singly or combined, demonstrated high degrees of reducing effects on AFM1 levels. Sterilization of the milk at 121?C and 80?C under the same condition of time (15 - 20) min showed significant reduction of up to 58.8% (p 0.05) in the level of AFM1 when compared with the initial mean AFM1 concentration of the untreated fresh milk. The situation was however different around the boiling temperature of 100?C at which point the level of AFM1 reduction was found to be inconsistent. The indigenized combined strains showed some slight margins of AFM1 reduction in the proportions of (20.5, 30.8 and 43.9)% over and above that of the exotic strains (17.4, 30.0 and 41.1)% in 12 h, 48 h and 72 h of fermentation respectively. Generally, fermentation alone showed lower reduction of AFM1 in milk from 24.5% to 43.9% compared with the reducing activities of (35.4 to 58.8)% when heat-treated milk samples were subsequently subjected to varied fermentation conditions.
基金the financial support provided by Fundacao para a Ciência e a Tecnologia,Portugal(PTDC/DTP-FTO/1057/2012)
文摘A simple, accurate and sensitive high-performance liquid chromatography （HPLC） method was developed, validated and applied to the determination of either theophylline or paracetamol in milk-based samples. The method allowed drug quantification in fresh and powdered milk with a relatively short run time of analysis and it was also successfully applied to the quantification of the drugs in solid dosage forms intended for pediatric use. Moreover, the main significant advantages over other published works are the simplicity of the sample preparation, reduced assay time and sample loss. The method meets the International Conference on Harmonization guideline for analytical methods validation regarding specificity, linearity, accuracy, precision, specificity and robustness as required by health authorities and applied by industry while designing and marketing new drug products. The technique encompasses the separation of the analytes with a reverse phase C18 column under isocrafic conditions and UV detection at 272 nm and 243 nm, respectively, for theophylline and paraeetamol. The lower limit of quantification for both drugs was determined as 0.2 μg/mL and the between-batch accuracy was 99.7%. This HPLC method allows quantification of theophylline and paracetamol in milk matrices and it can be applied in the design, development and production of milk-based pediatric dosage forms.
文摘建立高效液相色谱-串联质谱法测定生鲜乳中氯霉素残留的方法。对GB 29688—2013《牛奶中氯霉素残留量的测定液相色谱-串联质谱法》中的测定方法进行优化。量取生鲜乳适量,加氯霉素-D_(5)内标工作液,经乙腈萃取后,5000 r/min离心,过OASIS Prime HLB柱,将所过溶液氮气吹干,水复溶,取下层水溶液层过0.22μm水系滤膜。将C_(18)柱作为液相色谱柱,按V_((乙腈))∶V_((水))=60:40体积比等度洗脱。结果表明,氯霉素在0.2~10.0μg/kg范围内有较好的准确度,相关系数均大于0.99,方法检测限0.05μg/kg,定量限都为0.2μg/kg,3个加标浓度(0.2、1.0、10.0μg/kg)的氯霉素的平均回收率为85.5%~116.0%,相对标准偏差为1.23%~8.16%。试验结果完全符合国家标准检测要求,适用于生鲜乳中氯霉素定性定量快速检测。
文摘The main objective of this study was to analyze the effect of bacterial content (CFU) and somatic cell count (SCC) in milk quality in sheep (Ovis aries) farms according to the existing standards for fresh milk quality in Kosovo. A total of 2256 milk test day records from 379 Bardhoka (BAR), Sharri sheep (SHA), Kosovo sheep (KOS) and Balusha (BAL) ewes in eight herds across the country were collected and analyzed through a period April-October 2010. The general linear model and Duncan’s test were used to analyze the effect of different variables on presence of CFU and SCC in fresh milk. The effect of all variables was considered as a fixed. The overall results show that farm (P 0422), respectively, had a significant effect on presence of SCC. For CFU farm (P 0422) and breed (P 1211.17 to 6425.76 CFU/mL and 846.07 to 2043.15 SCC/mL milk, respectively. Although the rate of fresh milk contamination with SCC tends to be relatively low compare with CFU, by all means both variables should not be underestimated bearing in mind that a high rate of them on fresh milk are negatively correlated with farmer’s profit, consumer food safety and overall animal health.
基金Supported by Science and Technology Open Cooperation Project of Henan Province(162106000017)Science and Technology People-benefiting Plan Project of Henan Province(152207110004)+1 种基金Major Science and Technology Program of Henan Province(16110051020)Puyang Science and Technology Plan Project(160215)
文摘In order to establish an HPLC-MS/MS method for detecting progesterone in raw milk,raw milk was extracted with methanol,and then determined by HPLC-MS/MS after the purification with a C18 solid phase extraction column. Qualitative determination was performed according to retention time and selective ion abundance ratio,and quantification was performed by external standard method. The results showed that progesterone had a good linear relation in the range of0. 1-5. 0 ng/ml,with a correlation coefficient of 0. 999 9. The detection limit of the established method was 0. 02 μg/kg,and the quantification limit was0. 04 μg/kg. In the standard addition range of 0. 1-5. 0 ng/ml,the recovery ranged from 79. 6% to 105. 1%,with relative standard deviation≤8. 9%. Compared with the industry standard,the detection limit and the quantification limit of the established method are significantly reduced,and the sensitivity of the method is enhanced,so this method is suitable for the detection of progesterone residue in fresh milk in pastures.
