油炸薯条中酚类抗氧化剂的高效液相色谱法测定

采用反相高效液相色谱法测定油炸薯条中PG、TBHQ、BHA、4HR、BHT、2246.其中PG、TBHQ用50%甲醇(体积分数1%的冰醋酸)作流动相,BHA、4HR、BHT、2246用80%的甲醇作流动相,检测波长为280nm,用纯甲醇提取样品中的PG、TBHQ;用甲醇∶二氯甲烷=9∶ 1(V/V)提取BHA、4HR、BHT、2246.相关系数在0.9983～0.9996之间,检出限为1.0～2.0μg/g ,标准偏差在0.21%～5.30%之间,平均回收率均在85%以上.     

油炸薯条中酚类抗氧化剂的高效液相色谱法测定

采用反相高效液相色谱法测定油炸薯条中PG、TBHQ、BHA、4HR、BHT、2246。其中PG、TBHQ用50%甲醇(体积分数1%的冰醋酸)作流动相,BHA、4HR、BHT、2246用80%的甲醇作流动相,检测波长为280nm,用纯甲醇提取样品中的PG、TBHQ;用甲醇∶二氯甲烷=9∶1(V/V)提取BHA、4HR、BHT、2246。相关系数在0.9983~0.9996之间,检出限为1.0~2.0μg/g,标准偏差在0.21%~5.30%之间,平均回收率均在85%以上。      

高效液相色谱法测定15种蔬菜中的β-胡萝卜素

应用高效液相色谱法测定国内常用的15种蔬菜中β-胡萝卜素含量。蔬菜中的β-胡萝卜素经超声提取,用Kromasil C18(4.6mm×300mm,5μm)色谱柱,甲醇-四氢呋喃(THF)-2,6-二叔丁基-4-甲基苯酚(BHT)(9:1:0.01,V/V)为流动相,紫外检测器检测,检测波长为4 4 8 n m。结果表明,β-胡萝卜素出峰时间短(21 m in),检出限低(0.075μg/mL),在1～50μg/mL质量浓度范围内线性关系良好(R2=0.9997),平均加标回收率达97.84%(n=5)。该方法可避免β-胡萝卜素在预处理过程中被氧化,重复性好、操作简便、结果可靠,可用于多种新鲜蔬菜中β-胡萝卜素含量的测定。     

LC-MS/MS法测定浓缩果汁中2-氨基苯并咪唑、多菌灵、噻菌灵、甲基硫菌灵的残留量

建立了同时测定浓缩果汁中2-氨基苯并咪唑、噻菌灵、多菌灵、甲基硫菌灵的LC-MS/MS检测法。选取苹果、芒果、菠萝、梨、橙、荔枝、西番莲7种浓缩果汁进行了研究,样品采用乙腈提取,经PSA(乙二胺基N-丙基柱)柱净化后用LC-MS/MS测定。色谱条件是以甲醇-10mmol/L的乙酸铵(含0.1%体积浓度的甲酸)为流动相进行梯度洗脱,待测物经ZORBAX Eclipse XDB-C18柱分离,最后用电喷雾正离子(ESI+)和多反应监测模式(MRM)进行MS测定。结果表明,当2-氨基苯并咪唑添加水平为2、4、20μg/kg,噻菌灵、多菌灵、甲基硫菌灵添加水平为1、2、10μg/kg时,回收率为70.3%～109.8%,相对标准偏差为0.1%～10.9%,方法的检出限:2-氨基苯并咪唑2μg/kg、多菌灵1μg/kg、噻菌灵1μg/kg、甲基硫菌灵1μg/kg。该方法能有效检测出浓缩果汁中四种杀菌剂的残留量,且稳定性好,结果可靠,为监控浓缩果汁的质量安全提供了一个行之有效的途径。     

UPLC-MS/MS法测定猪肉及其制品中己烯雌酚残留量

以叔丁基甲醚为提取剂建立一种简单、快速的测定猪肉中己烯雌酚残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)法。样品经12 mL叔丁基甲醚分2次振荡提取,正己烷除脂,经SPE柱净化后,用7 mL甲醇-叔丁基甲基醚(1︰9, V/V)溶液洗脱,浓缩后,用2 mL 80%乙腈复溶,在电喷雾负离子模式下以多反应监测模式扫描检测,采用同位素内标法定量。结果表明:己烯雌酚分别在5～100μg/kg和100～1 000μg/kg质量分数范围内呈现良好的线性关系,相关系数r分别为0.999 4和0.999 8;在10, 50, 100和500μg/kg 4个添加水平下的空白加标回收率为86.3%～107.6%,相对标准偏差(S_RSD)为2.6%～12.4%。利用该法对猪肉粉质控样品(产品编号PKL04011305970B,参考值2.28 mg/kg,参考范围1.85～2.71 mg/kg)进行7次平行测定,其回收率为89.7%, S_RSD为2.7%。     

固相萃取-高效液相色谱检测鸡蛋中氟虫腈及其代谢物

目的建立固相萃取-高效液相色谱法测定鸡蛋中氟虫腈农药及其主要的代谢物氟虫腈砜、氟虫腈亚砜、氟甲腈的分析方法。方法选用含1%甲酸的乙腈溶液(V:V)为提取溶剂,用石墨化碳黑/氨基固相萃取小柱萃取净化,用乙腈作洗脱剂,并在以甲醇-水(67:33,V:V)为流动相的条件下进行高效液相色谱检测。结果该方法的线性范围为0.3～10.0μg/g,4种目标物的检测限均在0.05～0.10μg/g之间。通过对实际鸡蛋样品加标检测,得到加标回收率在80.9%～115.8%之间,相对标准偏差均小于6.2%。结论该方法精密度较高、稳定性良好、操作简便,可用于鸡蛋样品中氟虫腈及其3种代谢物的测定。     

免疫亲和柱净化-高效液相色谱柱后光化学衍生- 荧光检测器检测食品中黄曲霉毒素

目的建立一种免疫亲和固相萃取柱净化-高效液相色谱柱后光化学衍生-荧光检测器同时测定食品中黄曲霉毒素B_1、B_2、G_1和G_2的方法。方法以甲醇-水(70:30,V:V)为提取溶剂,采用高速均质提取,并经过黄曲霉毒素免疫亲和柱净化。结果经月旭公司Welch Ultimate~XB-C_(18)色谱柱(250 mm×4.6 mm,5μm)分离后使用光化学衍生器进行柱后衍生,并采用带荧光检测器的高效液相色谱仪检测,流动相为甲醇/水(45:55,V:V)。黄曲霉毒素B_1、B_2、G_1和G_2线性范围在0.3~50.0μg/L之间,线性相关系数均大于0.999,B_1、B_2、G_1和G_2检出限分别为0.15μg/kg、0.05μg/kg、0.15μg/kg、0.05μg/kg。在3个加标浓度下大米、花生和瓜子等试样的回收率在80.7%~92.6%之间;相对标准偏差(RSD)在2.04~3.87%之间。结论该方法的灵敏度、准确度和精密度均符合黄曲霉毒素的检测技术要求,且简便快速,适用于食品中黄曲霉毒素B_1,B_2,G_1和G_2的准确测定。     

基质固相分散-液相色谱法测定火腿肠中酚类环境雌激素

硅酸镁(florisil)作固相分散剂与样品混合,正己烷脱油脂,二氯甲烷洗提三种酚类环境雌激素,高效液相色谱法测定。色谱条件为:Diamonsil C18色谱柱(5μm,250mm×4.6mm),乙腈-甲醇-水(20:43:37,V/V)为流动相,甲酸调节pH=5。双酚A、己烯雌酚、己二烯雌酚在0.0005～0.1mg/ml之间均呈良好线性关系,样品检出限分别为0.05、0.1、0.05μg/g(S/N=3),相对标准偏差(RSD)低于4.5%,回收率80%以上。     

高效液相色谱法检测保健食品中的番茄红素

目的建立高效液相色谱法测定保健食品中番茄红素的分析方法。方法用含有0.1%2,6-二叔丁基-4-甲基苯酚抗氧化剂的甲醇:二氯甲烷(10:90,V:V)作为提取溶液。通过Agilent Eclipse XDB-C_(18)(4.6 mm×250mm,5μm)色谱柱;甲醇:乙酸乙酯(85:15,V:V)作为流动相,二极管阵列检测器,检出波长475 nm,色谱柱温25℃,流速1.0 mL/min,进样体积10μL,作为检测条件。结果番茄红素在0~200μg/mL范围内线性良好,相关系数r=0.9995,最低检出限为0.0815μg/mL,平均回收率在89.7%~109.8%之间,RSD为8.4%。结论本方法可以准确、快速地检测保健食品中的番茄红素。     

固相萃取-高效液相色谱-串联质谱法测定酱油中4-甲基咪唑

建立固相萃取-高效液相色谱-串联质谱/质谱法(SPE-HPLC-MS/MS)测定酱油中4-甲基咪唑的分析方法。试样经水稀释提取,LC-SCX固相萃取柱净化后,以乙腈和5mmol/L乙酸铵溶液(含0.1%甲酸,V/V)作为流动相,C18色谱柱分离,采用电喷雾离子源,正离子扫描多反应监测(MRM)模式进行检测。4-甲基咪唑在5~500μg/L浓度范围内呈良好线性关系,相关系数(r2)大于0.99,加标回收率为83.6%~95.1%,相对标准偏差为7.3%~8.2%,方法检出限为5μg/kg,定量限为10μg/kg。方法简单快速、准确灵敏,适用于酱油中4-甲基咪唑的测定。     

抗氧化剂的超高效液相色谱-串联质谱法测定

研究了油炸食品中化学合成酚类抗氧化剂--丁基羟基茴香醚(BHA)、二叔丁基对甲酚(BHT)、没食子酸丙酯(PG)、特丁基对苯二酚(TBHQ)的检测,采用超高效液相色谱-串联质谱法测定,以反相C18为分离柱,乙腈-甲醇水体系为流动相进行梯度洗脱,采用负离子检测模式,外标法定量。4种抗氧化剂呈良好线性关系(R2=0.9953~0.9998),PG方法检出限为2.0μg/kg,BHA、TBHQ检出限为200μg/kg,BHT检出限为500μg/kg。回收率为79%~96%,相对标准偏差为0.9%~5.3%,方法准确、灵敏、重现性好,可用于油炸食品中抗氧化剂的检测。     

气相色谱法测定饼干中的抗氧化剂BHA、BHT与TBHQ

建立了气相色谱法同时测定饼干中的3种抗氧化剂丁基羟基茴香醚（BHA）、二丁基羟基甲苯（B肿）和特丁基对苯二酚（TBHQ）含量的方法。样品采用无水乙醇提取,经净化、离心后直接进样测定。试验得出方法最低检出限BHA和BHT为1．0mg／kg,TBHQ为2．0mg／kg,3种抗氧化剂加标回收率在86．70％-103．02％之间,相对偏差均小于3％,线性范围在2μg／mL-200μg／mL之间,相关系数均大于0．999。该方法简便、快速、稳定、可靠,适用于饼干中BHA、BHT和TBHQ含量的同时快速检测。     

Effectiveness of antioxidants on the stability of banana chips

The effectiveness of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in improving the stability of banana chips stored at 65°C were compared. Criteria used in the assessment of the stability of the chips included the determinations of peroxide, p-anisidine, acid and iodine values, E_1cm ^1% at 232 amd 268 nm and the C18:2/C16:0 ratio of oil extracted from banana chips. It was found that chips fried in refined, bleached and deodorised (RBD) olein containing BHA or BHT were more stable than chips fried in RBD olein without antioxidants. BHT was more effective than BHA in prolonging the shelf-life of of banana chips. The same order of effectiveness of the antioxidants was observed at 65°C and at room temperature (25°C).     

PSE-HPLC 法测定食品中叔丁基羟基茴香醚和2,6- 二叔丁基羟基甲苯

目的：建立测定食品中抗氧化剂叔丁基羟基茴香醚(BHA)和2,6- 二叔丁基羟基甲苯(BHT)加压溶剂萃取-高效液相色谱法(PSE-HPLC 法)。方法：采用正交试验对影响PSE 萃取效率的温度、压力、萃取溶剂、萃取时间进行优化,联合HPLC 进行测定,并确定分别以BHA 提取量、BHT 提取量以及总量为评价指标的最优条件。结果：PSE-HPLC 法测定BHT 和BHA 的相对标准偏差(RSD)为0.5%～3.1%,并且在1.0～200.0μg/mL 范围内色谱峰面积与组分质量浓度均有很好的线性相关性(r ≥ 0.9997),检出限为0.05μg/mL,在最优条件下的回收率为92.60%～97.80%。结论：PSE-HPLC 法简便、快速、效率高,方法的重现性、线性相关性以及检出限理想,适用于食品中BHT 和BHA 含量及两者总量的同时快速检测。     

PSE-GC法同时测定饼干中两种抗氧化剂

建立测定饼干中的2种抗氧化剂叔丁基对羟基茴香醚(BHA)和二丁基羟基甲苯(BHT)的加压溶剂萃取-气相色谱法(PSE-GC法).采用PSE法进行样品萃取,萃取液经中性氧化铝净化后,进行GC分析.PSE-GC法测定饼干中BHT和BHA的相对标准偏差(RSD)为0.5％～3.1％,并且在2.0 μg/mL～200.0 μg/mL范围内色谱峰面积与组分浓度均有很好的线性相关性(r≥0.9994),检出限为0.5 μg/mL,回收率为94.68％～96.80％.PSE-GC法简便、快速、效率高,方法的重现性、线性相关性以及检出限理想,适用于饼干中BHT和BHA含量的同时快速检测.     

Simultaneous voltammetric determination of phenolic antioxidants in food using a boron-doped diamond electrode

A method for the simultaneous determination of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in food was developed using square-wave voltammetry (SWV). The determination of these phenolic antioxidants was carried out using a cathodically pre-treated boron-doped diamond electrode (BDD) and an aqueous-ethanolic (30% ethanol, v/v) 10 mmol L⁻¹ KNO₃ solution (pH_cond. 1.5) as supporting electrolyte. In the SWV measurements using the BDD electrode, the oxidation peak potentials of BHA and BHT present in binary mixtures were separated by about 0.3 V. The attained detection limits for the simultaneous determination of BHA and BHT (0.14 and 0.25 μmol L⁻¹, respectively) are lower than the ones by voltammetric techniques reported in the literature. The proposed method was successfully applied in the simultaneous determination of BHA and BHT in food products, with results similar to those obtained using a high-performance liquid chromatography method, at a 95% confidence level.     

Antioxidant properties of Mediterranean spices compared with common food additives

In this study, the antioxidant properties of Mediterranean food spices (annatto, cumin, oregano, sweet and hot paprika, rosemary, and saffron) at 5% concentration and of common food additives (butylated hydroxyanisole [BHA], butylated hydroxytoluene [BHT], and propyl gallate) at 100 microg/g are compared. The ability of these compounds to inhibit lipid peroxidation was, in decreasing order, rosemary > oregano > propyl gallate > annatto > BHA > sweet paprika > cumin > hot paprika > saffron > BHT. Deoxyribose damage is partially inhibited in the presence of cumin extract that exhibits the strongest protective action. The rest of the spices also protect deoxyribose better than the BHA and BHT used in the assay. Finally, the results obtained in the assay point to the prooxidant effect of propyl gallate. Hydrogen peroxide scavenging activity is measured by using peroxidase-based assay systems. In aqueous medium, the spice extracts show lower antioxidant activity than propyl gallate, the decreasing order being cumin > oregano > annatto > rosemary > hot paprika > sweet paprika. BHA and BHT did not scavenge H2O2 Spices are able to scavenge HOCl and protect alpha1-antiproteinase. The results indicate that rosemary and oregano are more effective HOCl scavengers than the other substances analyzed, which, in decreasing order, were propyl gallate, annatto, sweet and hot paprika, saffron, and cumin. The effect of Mediterranean food spices on the oxidative stability of refined olive oil tested by the Rancimat method was compared with common food additives during storage (72 h, 2, 4, and 6 months) at room temperature. The results showed that the spice extracts analyzed have significant stabilizing effects (P < 0.05).     

GC-MS法同时检测葡萄酒中10种防腐剂和抗氧化剂

利用离子阱气相色谱-质谱联用仪,优化了色谱、质谱仪器参数,利用质谱全扫描技术建立了同时检测葡萄酒中山梨酸、苯甲酸、脱氢乙酸、叔丁基对苯二酚（TBHQ）、叔丁基羟基茴香醚（BHA）、2,6-二叔丁基对甲酚（BHT）、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯等10种添加剂的方法。10种添加剂的检测限分别为0．11mg/L、0．072mg／L、0．046mg／L、0．035mg／L、0．032mg／L、0．020mg／L、0．035mg／L、0．042mg／L、0．035mg,／L、0．035mg／L,方法的精密度为2．9％～4．6％、回收率为82％～101％,应用于葡萄酒中食品添加剂的检测,效果良好,检测效率大大提高。     

In vitro determination of antioxidant activity of proteins from jellyfish Rhopilema esculentum

In this study, the antioxidant activity of proteins isolated from jellyfish, Rhopilema esculentum Kishinouye (R. esculentum), was determined by various antioxidant assays, including superoxide anion radical-scavenging, hydroxyl radical-scavenging, total antioxidant activity, reducing power and metal chelating activity. Butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), α-tocopherol, vitamin C and mannitol were used as standards in those various antioxidant activities. The crude protein (CP) and the protein fractions isolated by Sephadex chromatography, first peak (FP) and second peak (SP), had very low reductive power and metal chelating abilities compared to EDTA, but they showed strong scavenging effects on the superoxide anion radical, hydroxyl radical and varying total antioxidant activity. FP and SP exhibited stronger scavenging effects on the superoxide anion radical than BHA, BHT or α-tocopherol. The EC₅₀ values of FP and SP were 6.12 and 0.88 μg/ml, respectively, while values EC₅₀ of BHA, BHT and α-tocopherol were 31, 61 and 88 μg/ml, respectively. CP, FP and SP showed far higher hydroxyl radical-scavenging activities than did vitamin C or mannitol. The EC₅₀ values of CP, FP and SP were 48.76, 45.42 and 1.52 μg/ml, but EC₅₀ values of vitamin C and mannitol were 1907 and 4536 μg/ml, respectively. In a β-carotene–linoleate system, SP and CP showed antioxidant activity, but lower than BHA. Of the three samples, SP had the strongest antioxidant activity. So, SP may have a use as a possible supplement in the food and pharmaceutical industries.     

Estimated daily intakes of butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and tert-butyl hydroquinone (TBHQ) antioxidants in Korea.

The study was conducted to establish the estimated daily intake (EDI) of antioxidants such as butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and tert-butyl hydroquinone (TBHQ) in Korea. The EDIs were obtained from two sources. One of the estimations was based on the analytical determination of BHA, BHT and TBHQ in 12 food categories (ten food categories for TBHQ) and on individual dietary intake data obtained from the National Health and Nutrition Survey in 1998 (n=11 525, age > 1 year). The other EDIs of BHA, BHT and TBHQ were based on the maximum permitted levels specified in national food standards in Korea and on individual dietary intake data obtained from the National Health and Nutrition Survey in 1998 (n=11 525, age > 1 year). To establish the EDIs based on the analytical determination and on individual dietary intake data, 133 food samples in 12 food categories were selected from the foods considered to be representative sources of BHA, BHT and TBHQ in the Korean diet. Selected samples were analysed by GC with FID. BHA was not detected in any of the samples analysed. BHT and TBHQ were detected in the samples, but the levels were significantly lower than their maximum limits. The EDIs1 of BHT, and TBHQ for average consumers were 0.0156(-3), and 0.0012(-3) mg kg(-1) body weight bw day(-1) and as a proportion of the ADI were 0.0052 and 0.0002%, respectively. For 95th percentile consumers, the EDIs of BHT and TBHQ were 0.0080 and 0.0006 mg kg(-1) bw day(-1), and as a proportion of the ADI were 2.67 and 0.09%, respectively. EDIs for BHA, BHT and TBHQ based on the maximum permitted levels and on individual dietary intake data were 0.04, 0.04 and 0.04 mg kg(-1) bw day(-1), respectively. The EDIs of BHA, BHT and TBHQ for average consumers ranged from 6.00 to 14.42% of the ADI of each antioxidant. According to these results, the EDIs of BHA, BHT and TBHQ in Korea were significantly lower than ADI of these antioxidants established by the JECFA.