高效液相色谱法测定鸡组织中尼卡巴嗪标识残留物

应用高效液相色谱法测定鸡组织中尼卡巴嗪标识残留物-- 4,4＇- 二硝基均二苯脲。试样经乙腈-0.5g/mL氢氧化钾溶液提取,正己烷脱脂净化,用高效液相色谱仪(C18 柱)分析,流动相为乙腈- 体积分数1% 乙酸溶液(53:47,V/V),流速1.0mL/min,紫外检测波长为350nm。对鸡肉、鸡肝和鸡蛋样品进行0.05～0.50mg/kg 的药物添加回收实验,4,4＇- 二硝基均二苯脲的平均回收率为93.6%～102.0%(n=10),相对标准偏差为2.8%～10.4%,方法的定量限为0.05mg/kg。该法简便、准确,适用于鸡组织中尼卡巴嗪标识残留物4,4＇- 二硝基均二苯脲的检测。     

Determination method for ractopamine in swine and cattle tissues using LC/MS

Simple and reliable methods using LC/MS have been developed for the determination of the beta-agonist ractopamine in swine and cattle tissues. Ractopamine was extracted with ethyl acetate from muscle and liver, and the ethyl acetate layer was evaporated to dryness. The residue was purified by partition with acetonitrile/n-hexane. In the case of fat, ractopamine was extracted and purified by partition with acetonitrile/n-hexane. The resulting acetonitrile solutions were evaporated to dryness. The residue was dissolved in methanol, and subjected to LC/MS. The LC separation was performed on a Wakosil-II 3C18HG column (150 x 3 mm i.d.) in isocratic mode with 0.05% trifluoroacetic acid-acetonitrile (80:20) as a mobile phase at a flow rate of 0.4 mL/min. The MS detection was performed in the selected ion recording (SIR) mode, with detection of the M + H+ ion of ractopamine (m/z 302) produced by electrospray ionization (ESI). The mean recoveries of the drug from swine muscle (0.01 microg fortified), fat (0.01 microg fortified) and liver (0.04 microg/g fortified) were 99.7%, 99.5% and 100.8%, and those from cattle samples were 108.3%, 97.0% and 109.4%, respectively. The relative standard deviations (RSDs) ranged from 0.1% to 9.5%. The limit of quantification (LOQ) of the drug was 1 ng/g.     

Simultaneous determination of five antioxidants in food by HPLC with fluorescence detection

An HPLC method with fluorescence detection was developed for the determination of propyl gallate, nordihydroguaiaretic acid, butylated hydroxyanisole (2- and 3-tert-butyl-4-hydroxyanisole), tert-butylhydroquinone and octyl gallate in edible oils and foods. The antioxidants in edible oil were isolated directly with acetonitrile saturated with n-hexane. The antioxidants in food were extracted with ethyl acetate and the extract was concentrated under vacuum. They were isolated from the residue with acetonitrile saturated with n-hexane. The acetonitrile layer was centrifuged at 5,000 rpm for 10 min. The HPLC separation was performed on a Symmetry C18 column (3.5 microns, 4.6 mm i.d. x 150 mm) using a mixture of 5% acetic acid-acetonitrile-methanol (4:3:3, v/v/v) as the mobile phase and monitored by using a fluorescence detector with time programming. Sample peaks were identified by comparison of the fluorescence spectra with those of antioxidant standards. Average recoveries of fortified antioxidants at 100 micrograms/g were 72.1-99.6%. Coefficients of variation were 0.7-7.2%.     

Determination of benzimidazole anthelmintics in livestock foods by HPLC

A simple and rapid liquid chromatographic method was developed for the simultaneous determination of twelve benzimidazole anthelmintics in livestock foods using reversed-phase high-performance liquid chromatography with photodiode array detection (PDA). A sample was homogenized with acetonitrile and n-hexane, and centrifuged. The acetonitrile phase was isolated and evaporated. The residue was dissolved in 0.1 mol/L carbonate buffer solution (pH = 9.1), sonicated, and then subjected to clean-up on a Bond Elut LRC-C18 cartridge. The benzimidazole compounds were separated isocratically on a Capcell Pak C18 UG 120 (5 microns, 150 x 4.6 mm i.d.) column and detected by PDA at 295 and 313 nm. Mixtures of acetonitrile and 0.05 mol/L ammonium acetate in mixing ratios of (20:80) and (40:60) were used as the mobile phase, and the flow-rate was 1.0 mL/min at 40 degrees C. The mean recoveries (n = 3) from 0.1-0.5 microgram/g added samples were 72.6-97.2% with coefficients of variation of 0.3-8.5%. The detection limits were 0.01-0.05 microgram/g.     

高效液相色谱法同时测定食品中18种食品添加剂

建立高效液相色谱同时测定食品中18种食品添加剂的高通量分析方法。对于不含油脂或油脂含量低的样品采用含抗坏血酸棕榈酸酯的正己烷饱和乙腈-6mol/L HCl溶液-饱和氯化钠混合溶液一次提取净化,对于油脂样品采用含抗坏血酸棕榈酸酯的正己烷饱和乙腈-乙腈饱和正己烷液液萃取。采用Ecosil C18色谱柱(250mm×4.6mm,5μm),乙腈-0.6%乙酸溶液作为流动相,梯度洗脱,用紫外检测器检测,检测波长280nm,外标法峰面积定量。18种食品添加剂在1.0～25mg/L范围内线性良好,相关系数r均大于0.99,样品在10、25mg/kg和50mg/kg三个添加水平的平均回收率为88.9%～99.9%之间,相对标准偏差为2.43%～11.7%(n=6),方法的定量限为10mg/kg。方法简便、准确,适用于食品中18种食品添加剂高通量的检测。     

液相色谱-串联质谱法快速测定鸡肉及组织中的三聚氰胺和三聚氰酸

通过对提取溶剂、净化方法及色谱质谱条件的优化建立鸡组织样品中的三聚氰胺和三聚氰酸同时测定的HPLC-MS/MS 法。样品经乙腈水溶液(70:30,V/V)超声提取,正己烷脱脂,7000r/min 离心后取上清液与乙腈(1:1,V/V)混匀,10000r/min 离心沉淀蛋白,过滤后无需净化即可上机测定,大大缩短了样品处理时间。使用MRM模式检测和同位素内标稀释法定量,进一步提高了方法的准确性和定量线性。在1～500ng/mL 范围内,目标物的峰面积与其质量浓度的线性关系良好(R2 ＞ 0.999);在0.1、1、5mg/kg 的添加水平,鸡组织样品三聚氰胺回收率为87.76%～107.89%,三聚氰酸回收率为87.31%～106.05%,相对标准偏差(RSD)分别为0.58%～2.78% 和1.26%～4.33%;三聚氰胺和三聚氰酸的检测限(LOD)分别为4ng/g 和2ng/g。结果表明,该方法简便、快速、准确,适合鸡组织中三聚氰胺和三聚氰酸的确证和定量测定。     

Determination of nequinate and buquinolate in livestock products using liquid chromatography-tandem mass spectrometry

We studied the simultaneous determination of nequinate and buquinolate, which are used as feed additives to prevent coccidiosis, by means of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The sample was extracted with acetonitrile, then loaded onto an HLB mini-column with 20% methanol. After clean-up with 20% methanol, the analytes were eluted with acetonitrile-methanol (1 : 1). The coccidiostats in the purified samples were determined using ESI-MRM mode LC-MS/MS with a sample matrix calibration curve. Mean recoveries of nequinate and buquinolate from 8 kinds of livestocks samples (chicken muscle, chicken liver, chicken heart, swine muscle, swine heart, cattle muscle, sheep muscle, egg) were in the range of 89.5% to 108.6%, and the relative standard deviation values were <20% (n=10) at the levels of 0.01 μg/g and 0.05 μg/g, respectively. The limits of quantification of these compounds were 0.001 μg/g in each sample.     

Determination of glycarbylamide residues in chicken tissues by HPLC with post-column reaction

A newly developed HPLC method for determination of glycarbylamide (GB) in chicken liver was applied to other tissues (muscle, fat and kidney). The recoveries of GB in muscle, fat and kidney were 87.2% (CV 0.5), 91.3% (CV 4.7), 79.7% (CV 1.0), respectively. The detection limit of GB was 0.01 ppm. GB concentrations were determined by this method in tissues (muscle, fat, liver and kidney) from chickens sacrificed 5 days after oral administration of GB mixed in feed at 60 mg/kg of feed for 7 days. GB was not detected in these chicken tissues.     

Multi-residue method for determination of veterinary drugs and feed additives in meats by HPLC

A simple and rapid multi-residue method was developed for the determination of 28 kinds of veterinary drugs and feed additives (drugs) in muscle of cattle, pig and chicken. The drugs were extracted with acetonitrile-water (95:5) in a homogenizer and ultrasonic generator. The extracted solution was poured into an alumina column and the drugs were eluted with acetonitrile-water (90:10). The eluate was washed with n-hexane saturated with acetonitrile and then evaporated. The drugs were separated on a Inertsil ODS-3V column (4.6 mm i.d. x 250 mm) with a gradient system of 0.1% phosphoric acid-acetonitrile as the mobile phase, with monitoring at 280 and 340 nm. The recoveries of the 26 kinds of drugs were over 60% from the meats fortified at 0.1 microg/g, and the quantification limits of most drugs were 0.01 microg/g. This proposed method was found to be effective and suitable for the screening of the above drugs in meats.     

在线柱前衍生-高效液相色谱-荧光检测法测定牛奶中乙酰氨基阿维菌素残留量

目的建立一种在线柱前衍生-高效液相色谱-荧光检测法测定牛奶中乙酰氨基阿维菌素残留量。方法试样经饱和氯化钠水溶液盐析后,利用乙腈-二氯甲烷溶液提取,氮气吹干、10%(体积分数)N-甲基咪唑-乙腈溶液复溶、乙腈饱和正己烷多次净化。利用进样程序对净化后的溶液进行在线柱前衍生,高效液相色谱仪分离,荧光检测器检测,以保留时间定性,峰面积定量。结果结果表明,在25～400 ng/mL浓度范围内,标准曲线线性关系良好,相关系数r2大于0.999;该方法的回收率在94.8%～103.8%之间,相对标准偏差(relative standard deviation, RSD)均小于1.5。结论该方法非常简便,且具有较高的准确度、灵敏度和稳定性,适用于牛奶中乙酰氨基阿维菌素残留的检测。     

HPLC-MS/MS快速测定动物肌肉中6种聚醚类抗生素

建立动物肌肉组织中6种聚醚类抗生素(莫能菌素、马杜拉霉素、盐霉素、和拉沙洛菌素、甲基盐霉素、尼日利亚茵素)的高效液相色谱—电喷雾串联质谱快速测定法.样品经乙腈提取,并以乙腈饱和的正已烷净化,采用甲酸水溶液—甲醇体系为流动相,梯度洗脱,电喷雾离子源正离子多反应监测模式进行质谱分析.结果表明,在优化的条件下对样品进行分析检测,各抗生素的回收率为88.0％～108.7％,RSD为2.3％～6.1％(C=10μg/kg,n=5),6种待测物在1.0～150ng/mL范围内均呈线性,线性回归系数R2均大于0.99,检出限为0.05～0.2μg/kg.该方法操作简单,灵敏度高,适用于动物肌肉组织中6种聚醚类药物的批量检测分析.     

高效液相色谱- 串联质谱法快速测定鱼肉中4 种氟喹诺酮类药物残留

建立快速测定鱼肉中4 种氟喹诺酮类药物残留的高效液相色谱- 串联质谱方法。采用酸性乙腈提取样品中的氟喹诺酮药物残留,然后用正己烷脱脂,氮吹浓缩定容后,用反相液相色谱分离,以液相色谱- 串联质谱仪测定,外标法定量。该法对4 种氟喹诺酮类药物的线性范围为2～40μg/kg,相关系数(r2)大于0.997,在4、10、20μg/kg 3 个添加水平范围内的回收率为79.9%～98.1%,相对标准偏差为2.7%～8.7%,检出限为0.1～0.4μg/kg,定量限为0.3～1.0μg/kg。结果表明,该方法简便快速、灵敏度高、重现性好、选择性强,适用于鱼肉中氟喹诺酮类药物残留的定量测定。     

鸡蛋、鸡肉及奶粉中22种有机氯农药残留的测定

建立了在鸡蛋、鸡肉和奶粉中同时测定22种有机氯农药残留的方法。样品经乙腈提取、Captiva EMR-Lipid固相萃取柱净化、正己烷复溶后,用气相色谱仪检测,外标法定量。在0.005~0.2 mg/L范围内,22种有机氯农药的质量浓度与其对应的峰面积之间线性关系良好,R²均大于0.995。在0.01、0.02、0.1 mg/kg 3个添加水平下,重复测定6次,22种有机氯农药的回收率均在60%~110%,RSD均小于10%,符合GB 27404—2008的实验室内变异系数要求。该方法能够有效去除鸡蛋、鸡肉和奶粉中的动物脂肪及亲脂性干扰物,方法灵敏度、准确度和精密度均符合农药残留检测的要求,为有效监测鸡蛋、鸡肉和奶粉中有机氯农药残留量提供了一种高效、可靠的分析手段。     

鸡肉组织中氯羟吡啶残留超高效液相色谱检测方法研究

对鸡肉组织中氯羟吡啶残留高效液相色谱方法进行了研究,建立了鸡肉组织中氯羟吡啶残留超高效液相色谱检测方法。取鸡肉样品,用乙腈提取,正己烷脱脂,过氧化铝B 柱,用20ml 甲醇洗脱,减压蒸干,残留物用甲醇溶解,紫外检测器在267nm 波长下测定,流动相为乙腈:水(10:90,V/V)。氯羟吡啶浓度在10～1000μg/L 范围内,呈良好的线性,相关系数＞ 0.999,在10、50、100μg/kg 三个添加水平,平均回收率60.5%～94.6%,日内变异系数在4.2%～10.2%之间,日间变异系数在6.6%～12.7%之间,方法检测限为5μg/kg,定量限为15μg/kg。     

高效液相色谱法测定猪肉中氟喹诺酮类药物

采用高效液相色谱－荧光法（HPLC—FLD）柃测猪肉中两种氟喹诺酮类药物。猪肉样品经无水硫酸钠脱水后用1％醋酸＋乙腈提取,提取液用正己炕饱和的乙腈净化,用流动相（乙腈、0．01mol／L磷酸二氢钠（磷酸调pH3）体积比10：90）定容。通过对猪肉样品中氟喹诺酮类药物的检测表明该方法具有准确、快速、灵敏的特点。     

UPLC-MS/MS法同时测定牛奶中青霉素G及青霉噻唑酸

利用超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定牛奶中的青霉素G和青霉噻唑酸。样品经乙腈沉淀蛋白,上清液氮气吹干后,用水溶解,加入正己烷萃取除去脂肪;提取液经ACQUITYUPLCBEHC18柱分离,乙腈-1mmol/L乙酸铵+0.1%甲酸水溶液洗脱。青霉素G和青霉噻唑酸的检出限分别为1、2μg/kg,定量限分别为5、10μg/kg。在10～100ng/mL浓度范围内线性良好,相关系数均大于0.999,牛奶中的加标回收率在92%～103%,精密度(RSD,n=3)范围在2%～4%。     

植物油中叔丁基对苯二酚转化产物的识别确证与测定

目的:通过模拟日常生活中植物油加热的过程,确定了含有叔丁基对苯二酚（TBHQ）植物油样品中TBHQ转化降解的条件,采用气相色谱－质谱检测、未知化合物与数据库的匹配最终确定了TBHQ两种转化产物叔丁基对苯醌（TQ）、2,5-二叔丁基-1,4-苯醌（TBK）,并建立了植物油中TBHQ及其两种降解产物TQ、TBK气相色谱－质谱联用检测方法。方法:样品经乙腈饱和的正己烷溶解,正己烷饱和的乙腈提取,取乙腈层,提取两次,合并乙腈层,40 ℃水浴下减压浓缩至近干,甲醇复溶,采用HP-5MS UI毛细管柱（30 m×0.25 mm,0.25 μm）,不分流进样,选择离子监测模式,气相色谱－质谱仪测定,外标法定量。结果:3种化合物在各自浓度范围内线性良好（R2>0.995）,在3个加标水平下,平均回收率范围为83.40%～107.71%,相对标准偏差（n=6）小于8.50%。3种化合物定量限TBHQ和TBK为10 μg/kg,TQ为50 μg/kg,25批次样品测定,其中两批次样品测定出TQ,该样品经加热处理后均测定出TBK。结论:该方法操作简便,灵敏度高,准确可靠,适用于植物油中TBHQ及其降解产物的同时测定。     

Determination method of polysorbates in powdered soup by HPLC

A method for qualitative and quantitative analyses of polysorbates in powdered soup by HPLC was studied. Polysorbates in samples were extracted with acetonitrile after rinsing with n-hexane to remove fats and oils. The extract was cleaned up using a Bond Elut silica gel cartridge (500 mg). The cartridge was washed with ethyl acetate and polysorbates were eluted with a small amount of acetonitrile-methanol (1:2) mixture. The eluate was treated with cobalt thiocyanate solution to form a blue complex with polysorbate. In order to determine polysorbate, the complex was subjected to HPLC with a GPC column, using a mixture of acetonitrile-water (95:5) as a mobile phase, with a detection wavelength of 620 nm. The recoveries of polysorbate 80 added to powdered soups were more than 75% and the determination limit was 0.04 mg/g. When the proposed method was applied to the determination of polysorbates in 16 commercial samples of powdered soup for instant noodles and seasoning consomme, no polysorbates were detected in any sample.     

分子印迹固相萃取—高效液相色谱法检测鱼肉中的孔雀石绿和结晶紫

将分子印迹固相萃取和高效液相色谱法联用,建立一种检测鱼肉中孔雀石绿和结晶紫及其代谢产物残留的新方法。以孔雀石绿为模板分子,甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,本体聚合法合成分子印迹聚合物。并制成分子印迹固相萃取柱,优化分子印迹固相萃取的实验条件。鱼肉样品经过超声提取后,采用分子印迹固相萃取富集净化,用高...     

高效液相色谱法同时测定食品中的12种抗氧化剂

目的：建立一种快速、准确测定食品中12 种抗氧化剂的高效液相色谱法。方法：样品用正己烷溶解,用含抗坏血酸棕榈酸盐(AP)的饱和乙腈萃取,以反相C18 柱为分离柱,以甲醇- 乙腈- 乙酸- 水体系为流动相进行梯度洗脱,采用高效液相色谱- 紫外检测器于280nm 定量检测。结果：12 种抗氧化剂在36min 内完全分离,线性范围为0.2～200mg/L(r=0.9981～0.9999),定量限为0.2～1.0mg/kg,回收率为81.13%～107.57%,相对标准偏差为0.26%～4.52%(n=7)。结论：本方法准确、可靠、简便、检出限低,适合分析大批量样品。