RP-HPLC同时检测苹果浓缩汁中主要危害性指标方法的建立
|
摘要
随着苹果浓缩汁产业的发展,我国苹果浓缩汁所占比例日益增加,苹果汁出口贸易额逐年增长。然而,由于国际市场对食品安全的日益重视以及部分发达国家贸易保护主义的抬头,我国的农产品出口不断受到“绿色贸易壁垒”的困扰,苹果浓缩汁出口也不例外。
根据来自海关和商检的信息,我国苹果浓缩汁出口出现退货的主要原因有:部分产品不同程度出现乳酸、富马酸、5-羟甲基糠醛、展青霉素以及农药残留超标。这些个别指标的超标对我国苹果浓缩汁以及其他农产品的国际出口声誉均带来了不利的影响。因此,加强果汁安全因子多残留同时检测刻不容缓。
本研究在对苹果浓缩汁贸易中经常出现的超标指标进行系统研究的基础上,分别建立了RP-HPLC(reversed phase high-performance liquid chromatography,简称RP-HPLC)同时检测乳酸、富马酸、5-HMF和展青霉素;RP-HPLC同时检测乐果、多菌灵、5-HMF和展青霉素以及RP-HPLC同时检测11种不同类型农药的快速检测方法。以上检测方法的应用有利于保证我国苹果浓缩汁产品质量,使我国的苹果浓缩汁能顺畅进入国际市场。
本论文主要从以下六个方面进行了研究,并获得了相应的结论。
1.研究出5-HMF与展青霉素液.液萃取富集后再实现乳酸、富马酸适倍稀释的苹果浓缩汁样品预处理方法,为四组分的同时定量检测奠定了良好的基础。通过试验发现:本预处理方法对苹果浓缩汁中乳酸、富马酸、5-HMF以及展青霉素的回收率分别为95.65～99.91%、96.53～102.35%、89.96～101.33%、94.11～98.23%,CV<5%;方法的最低检出浓度为乳酸0.179mg·L~(-1)、富马酸3.217μg·L~(-1)、5-HMF5.672μg·L~(-1)和展青霉素8.90μg·L~(-1)。
2.建立同时分离检测乳酸、富马酸、5-HMF和展青霉素的双通道色谱分析方法,实现了该四组分的在不同检测波长下的同时检测。经过对流动相的组成比例、流速、柱温以及pH等条件的摸索,确立了在柱温30℃、流速1.00mL·min~(-1)的条件下,以pH2.5的磷酸水配制含5%L腈的混合溶液最为流动相,210nm和276nm同时检测该四组分的最佳色谱条件。所建立的标准曲线方程最低定量限分别为:乳酸0.597mg·L~(-1)、富马酸10.723μg·L~(-1)、5-HMF18.907μg·L~(-1)以及展青霉素29.667μg·L~(-1)。10次进样的保留时间CV<0.5%。
3.确定了同时检测5-HMF、展青霉素、乐果以及多菌灵的液-液萃取样品预处理方法。其流程是乙酸乙酯萃取-碱液净化-酸液强化。该方法对苹果浓缩汁中四组分的回收率分别为:乐果89.62～98.35%、多菌灵89.55～99.91%、5-HMF95.62～101.33%以及展青霉素85.65～95.72%。
4.建立了同时分离检测乐果、多菌灵、5-HMF和展青霉素的双通道色谱分析方法,实现了该四组分的在不同检测波长下的同时检测。通过对流动相组成比例的研究,认为以甲醇:乙腈:水=1:1:8为流动相,流速0.8mL/min,柱温30℃进行210nm检测乐果和多菌灵同时在276nm检测5-HMF和展青霉素的色谱分离方法最为理想。各组分的最低定量限分别为:5-HMF0.04869mg·L~(-1)、展青霉素0.0207mg·L~(-1)、多菌灵0.5801mg·L~(-1)和乐果0.0922mg·L~(-1)。10次进样的保留时间CV<1%。
5.研究出基于SPE-C_(18)同时富集苹果浓缩汁中11种农药组分的样品预处理方法。通过对净化液组成、净化液使用量、洗脱液使用量等因素的研究,实现了11种不同类型农药的同时富集。加标回收率测试结果表明:11种农药的加标回收率为86.27%～103.66%。
6.建立了同时分离检测苹果浓缩汁中11种不同类型农药残留的色谱分析方法。通过对流动相组成比例以及流动方式的研究,建立了以乙腈:水=55:45的混合液为流动相的不等速洗脱方法,实现了苹果浓缩汁贸易中常见11种农药残留的同时分离检测,并建立了特定色谱条件下11种农药残留组分的标准曲线。各组分的最低检测限测试结果表明:该色谱分析方法可以满足国内外农药残留检测的要求。
With the development of the world's apple juice concentrate industry,the proportion of China's apple juice concentrate is increasing year by year and export trade is becoming biger and biger. However,due to peoples pay attention to the food security increasingly,as well as the "trade protectionism" increased in some developed countries,China's exports of agricultural products is falling into the "green barriers" trouble and the export of China's apple juice concentrate is limited too.
According to the statistics from customs and institution of commodity inspection,the main reason of repercussion of Chinese apple juice concentrate exports is that some indicators such as lactic acid,fumaric acid,5-HMF,patulin and pesticide residues exceeded the standard.These occurrences impacted other agricultural exports as well as reputation of China's international exports.Therefore,it is necessary to put quality of the fruit juice into practice immediately.
On the basis of study on the indicators exceeded standards of apple juice concentrate systematically,three RP-HPLC methods have been established:1) to determine lactic acid,fumaric acid,5-HMF and patulin simultaneously by RP-HPLC.2) to determine dimethoate,carbendazol, 5-HMF,patulin simultaneously by RP-HPLC.3) to determine 11 different types of pesticides simultaneously by RP-HPLC.The purpose of this study is to ensure China's apple juice concentrate product quality and safety,break through the technological barriers and make China's apple juice concentrate enter the international market smoothly.
The study of this paper mainly focus on the following of six aspects and the corresponding conclusions were obtained.
1.A new method of sample pretreatmentis has been developed,which can enrich 5-HMF and patulin by liquid-liquid extraction and can dilute lactic acid and fumaric acid properly.It makes a good foundation for the four components of the quantitative detection.The results shows that:lactic acid,fumaric acid,5-HMF and patulin recoveries were 95.65-99.91%,96.53-102.35%, 89.96-101.33%,94.11-98.23%respectively and CV＜5%.The lowest detectable concentration of them are lactic acid 0.179mg·L~(-1),fumaric acid 3.217μg·L~(-1),5-HMF5.672μg·L~(-1) and patulin 8.90μg·L~(-1) for the method of sample pretreatment in apple juice concentrate respectively.
2.A new chromatographic method has been developed that is based on technique of dual pathways to separate and detect four materials including lactic acid(210nm),fumaric acid(210nm), 5-HMF(276nm),patulin(276nm) simultaneously.After studied mobile phase's composition, proportion,flow rate,pH and temperature of chromatographic column,the best chromatographic condition has been established that is the mixture phosphoric acid solution(pH 2.5)-acetonitrile (95:5,v/v) as the mobile phase with a flow rate of 1.00 ml·min~(-1) at 30℃.Limit of quantitation of them are lactic acid 0.597mg·L~(-1),fumaric acid 10.723μg·L~(-1),5-HMF18.907μg·L~(-1) and patulin 29.667μg·L~(-1),CV of retention time for 10 vices＜0.5%.
3.A new method of sample pretreatment has been developed that could enrich 5-HMF,patulin, dimethoate and carbendazol through the path including acetoacetate extracting—lye purifying—acidizing fluid potentizing.The results show that:dimethoate,carbendazol,5-HMF and patulin recoveries were 89.62-98.35%,89.55-99.91%,95.62-101.33%,85.65-95.72%respectively.
4.A new chromatographic method has been developed that is based on technique of dual pathways to separate and detect four componentes(dimethoate,carbendazol,5-HMF,patulin) simultaneously.After studied mobile phase's proportion,the best chromatographic condition has been established that is the mixture methanol-acetonitrile-water(1:1:8,v/v) as the mobile phase with a flow rate of 0.80 ml·min~(-1) at 30℃.In this condition,dimethoate and carbendazoi will be detected at 210nm while 5-HMF and patulin will be detected at 276nm.The standard curve of four components shows that limit of quantitation are 5-HMF 0.04869mg·L~(-1),patulin 0.0207mg·L~(-1),carbendazol 0.5801mg·L~(-1) and dimethoate 0.0207mg·L~(-1),CV of retention time for 10 vices＜1%.
5.Based on solid phase extraction,a new method(SPE-C_(18)) of sample pretreatment has been developed to enrich 11 kinds of pesticides,by studing the composition,dosis of purifying liquid and dosis of eluent.Test of recoveries shows that recoveries of 11 kinds of pesticides were between 86.27%and 103.66%.
6.A new chromatographic method has been developed to separate and detect 11 kinds of pesticides simultaneously.After studied mobile phase's composition,proportion and mode of flow rate,the best chromatographic condition has been established that is the mixture water-acetonitrile (45:55,v/v) as the mobile phase with a changed flow rate at 30℃.Standard curve of 11 kinds of pesticides has been developed.Resultes of lowest detectable limit shows that this method could be fit for detection requirement of pesticide residue.
根据来自海关和商检的信息,我国苹果浓缩汁出口出现退货的主要原因有:部分产品不同程度出现乳酸、富马酸、5-羟甲基糠醛、展青霉素以及农药残留超标。这些个别指标的超标对我国苹果浓缩汁以及其他农产品的国际出口声誉均带来了不利的影响。因此,加强果汁安全因子多残留同时检测刻不容缓。
本研究在对苹果浓缩汁贸易中经常出现的超标指标进行系统研究的基础上,分别建立了RP-HPLC(reversed phase high-performance liquid chromatography,简称RP-HPLC)同时检测乳酸、富马酸、5-HMF和展青霉素;RP-HPLC同时检测乐果、多菌灵、5-HMF和展青霉素以及RP-HPLC同时检测11种不同类型农药的快速检测方法。以上检测方法的应用有利于保证我国苹果浓缩汁产品质量,使我国的苹果浓缩汁能顺畅进入国际市场。
本论文主要从以下六个方面进行了研究,并获得了相应的结论。
1.研究出5-HMF与展青霉素液.液萃取富集后再实现乳酸、富马酸适倍稀释的苹果浓缩汁样品预处理方法,为四组分的同时定量检测奠定了良好的基础。通过试验发现:本预处理方法对苹果浓缩汁中乳酸、富马酸、5-HMF以及展青霉素的回收率分别为95.65～99.91%、96.53～102.35%、89.96～101.33%、94.11～98.23%,CV<5%;方法的最低检出浓度为乳酸0.179mg·L~(-1)、富马酸3.217μg·L~(-1)、5-HMF5.672μg·L~(-1)和展青霉素8.90μg·L~(-1)。
2.建立同时分离检测乳酸、富马酸、5-HMF和展青霉素的双通道色谱分析方法,实现了该四组分的在不同检测波长下的同时检测。经过对流动相的组成比例、流速、柱温以及pH等条件的摸索,确立了在柱温30℃、流速1.00mL·min~(-1)的条件下,以pH2.5的磷酸水配制含5%L腈的混合溶液最为流动相,210nm和276nm同时检测该四组分的最佳色谱条件。所建立的标准曲线方程最低定量限分别为:乳酸0.597mg·L~(-1)、富马酸10.723μg·L~(-1)、5-HMF18.907μg·L~(-1)以及展青霉素29.667μg·L~(-1)。10次进样的保留时间CV<0.5%。
3.确定了同时检测5-HMF、展青霉素、乐果以及多菌灵的液-液萃取样品预处理方法。其流程是乙酸乙酯萃取-碱液净化-酸液强化。该方法对苹果浓缩汁中四组分的回收率分别为:乐果89.62～98.35%、多菌灵89.55～99.91%、5-HMF95.62～101.33%以及展青霉素85.65～95.72%。
4.建立了同时分离检测乐果、多菌灵、5-HMF和展青霉素的双通道色谱分析方法,实现了该四组分的在不同检测波长下的同时检测。通过对流动相组成比例的研究,认为以甲醇:乙腈:水=1:1:8为流动相,流速0.8mL/min,柱温30℃进行210nm检测乐果和多菌灵同时在276nm检测5-HMF和展青霉素的色谱分离方法最为理想。各组分的最低定量限分别为:5-HMF0.04869mg·L~(-1)、展青霉素0.0207mg·L~(-1)、多菌灵0.5801mg·L~(-1)和乐果0.0922mg·L~(-1)。10次进样的保留时间CV<1%。
5.研究出基于SPE-C_(18)同时富集苹果浓缩汁中11种农药组分的样品预处理方法。通过对净化液组成、净化液使用量、洗脱液使用量等因素的研究,实现了11种不同类型农药的同时富集。加标回收率测试结果表明:11种农药的加标回收率为86.27%～103.66%。
6.建立了同时分离检测苹果浓缩汁中11种不同类型农药残留的色谱分析方法。通过对流动相组成比例以及流动方式的研究,建立了以乙腈:水=55:45的混合液为流动相的不等速洗脱方法,实现了苹果浓缩汁贸易中常见11种农药残留的同时分离检测,并建立了特定色谱条件下11种农药残留组分的标准曲线。各组分的最低检测限测试结果表明:该色谱分析方法可以满足国内外农药残留检测的要求。
With the development of the world's apple juice concentrate industry,the proportion of China's apple juice concentrate is increasing year by year and export trade is becoming biger and biger. However,due to peoples pay attention to the food security increasingly,as well as the "trade protectionism" increased in some developed countries,China's exports of agricultural products is falling into the "green barriers" trouble and the export of China's apple juice concentrate is limited too.
According to the statistics from customs and institution of commodity inspection,the main reason of repercussion of Chinese apple juice concentrate exports is that some indicators such as lactic acid,fumaric acid,5-HMF,patulin and pesticide residues exceeded the standard.These occurrences impacted other agricultural exports as well as reputation of China's international exports.Therefore,it is necessary to put quality of the fruit juice into practice immediately.
On the basis of study on the indicators exceeded standards of apple juice concentrate systematically,three RP-HPLC methods have been established:1) to determine lactic acid,fumaric acid,5-HMF and patulin simultaneously by RP-HPLC.2) to determine dimethoate,carbendazol, 5-HMF,patulin simultaneously by RP-HPLC.3) to determine 11 different types of pesticides simultaneously by RP-HPLC.The purpose of this study is to ensure China's apple juice concentrate product quality and safety,break through the technological barriers and make China's apple juice concentrate enter the international market smoothly.
The study of this paper mainly focus on the following of six aspects and the corresponding conclusions were obtained.
1.A new method of sample pretreatmentis has been developed,which can enrich 5-HMF and patulin by liquid-liquid extraction and can dilute lactic acid and fumaric acid properly.It makes a good foundation for the four components of the quantitative detection.The results shows that:lactic acid,fumaric acid,5-HMF and patulin recoveries were 95.65-99.91%,96.53-102.35%, 89.96-101.33%,94.11-98.23%respectively and CV＜5%.The lowest detectable concentration of them are lactic acid 0.179mg·L~(-1),fumaric acid 3.217μg·L~(-1),5-HMF5.672μg·L~(-1) and patulin 8.90μg·L~(-1) for the method of sample pretreatment in apple juice concentrate respectively.
2.A new chromatographic method has been developed that is based on technique of dual pathways to separate and detect four materials including lactic acid(210nm),fumaric acid(210nm), 5-HMF(276nm),patulin(276nm) simultaneously.After studied mobile phase's composition, proportion,flow rate,pH and temperature of chromatographic column,the best chromatographic condition has been established that is the mixture phosphoric acid solution(pH 2.5)-acetonitrile (95:5,v/v) as the mobile phase with a flow rate of 1.00 ml·min~(-1) at 30℃.Limit of quantitation of them are lactic acid 0.597mg·L~(-1),fumaric acid 10.723μg·L~(-1),5-HMF18.907μg·L~(-1) and patulin 29.667μg·L~(-1),CV of retention time for 10 vices＜0.5%.
3.A new method of sample pretreatment has been developed that could enrich 5-HMF,patulin, dimethoate and carbendazol through the path including acetoacetate extracting—lye purifying—acidizing fluid potentizing.The results show that:dimethoate,carbendazol,5-HMF and patulin recoveries were 89.62-98.35%,89.55-99.91%,95.62-101.33%,85.65-95.72%respectively.
4.A new chromatographic method has been developed that is based on technique of dual pathways to separate and detect four componentes(dimethoate,carbendazol,5-HMF,patulin) simultaneously.After studied mobile phase's proportion,the best chromatographic condition has been established that is the mixture methanol-acetonitrile-water(1:1:8,v/v) as the mobile phase with a flow rate of 0.80 ml·min~(-1) at 30℃.In this condition,dimethoate and carbendazoi will be detected at 210nm while 5-HMF and patulin will be detected at 276nm.The standard curve of four components shows that limit of quantitation are 5-HMF 0.04869mg·L~(-1),patulin 0.0207mg·L~(-1),carbendazol 0.5801mg·L~(-1) and dimethoate 0.0207mg·L~(-1),CV of retention time for 10 vices＜1%.
5.Based on solid phase extraction,a new method(SPE-C_(18)) of sample pretreatment has been developed to enrich 11 kinds of pesticides,by studing the composition,dosis of purifying liquid and dosis of eluent.Test of recoveries shows that recoveries of 11 kinds of pesticides were between 86.27%and 103.66%.
6.A new chromatographic method has been developed to separate and detect 11 kinds of pesticides simultaneously.After studied mobile phase's composition,proportion and mode of flow rate,the best chromatographic condition has been established that is the mixture water-acetonitrile (45:55,v/v) as the mobile phase with a changed flow rate at 30℃.Standard curve of 11 kinds of pesticides has been developed.Resultes of lowest detectable limit shows that this method could be fit for detection requirement of pesticide residue.
引文
[1]尤建强,崔岩.对我国水果进出口贸易的思考[J].国际贸易问题,2006,6:26-31.
[2]白志礼,穆养民,赵政阳.陕西苹果产业发展的新思考与新探索[J].干旱地区农业研究,2003,21(4):172-175.
[3]赵政阳,冯宝荣,王雷存,王章陵,周卫国.我国苹果产业向优势区域集中的战略思考[J].西北农业学报,2004,13(4):195-199.
[4]赵贵宝.我国苹果浓缩汁加工出口的形势、问题与对策[J].陕西农业科学,2004,5:63-66.
[5]张敬滋.我国小苹果做出世界大文章-中国苹果浓缩汁行业发展概况综述[J].农村实用工程技术.农业产业化,2004,2:35-38.
[6]仇农学,肖旭霖,邓红.陕西省苹果浓缩汁行业可持续发展的战略思考[J].农业工程学报,2000,16(1):122-124.
[7]成喜玲.陕西苹果汁加工业存在的问题及其对策[J].陕西省行政学院.陕西省经济管理干部学院学报,2005,19(2):43-46.
[8]解维域.苹果浓缩汁中若干重要质量指标的检测与控制[J].我国果菜,2001,3:25.
[9]柳畅先,庹浔,吴士筠.酶法测定乳酸[J].分析试验室,2005,24(9):75-77.
[10]V.Galli,C.Barbas.Capillary electrophoresis for the analysis of short-chain organic acids in coffee[J].Journal of Chromatography A,2004,1032(1-2) 1:299-304.
[11]王俊华,杨洁,申彤.乳酸发酵胡萝卜汁中有机酸的HPLC测定[J].现代食品科技,2006,4:235-238.
[12]章新,朱惠贤,王林,杨光宇,胡秋芬.用快速分离柱高效液相色谱法测定生物发酵产物中的乳酸[J].我国酿造,2005,7:53-54.
[13]汤丽芬,吴珏珩,张选红,陈健文,陈红英,林广云.高效液相色谱法同时测定小鼠脑组织中乳酸与磷酸肌酸含量[J].中国卫生检验杂志,2005,15(3):300-302.
[14]朱振宝,田呈瑞,易建华,朱粉莉.苹果汁中富马酸的吸附[J].陕西科技大学学报,2001,21(3):36-39.
[15]陈爱华,焦必宁.常见果汁掺假检测技术的研究进展[J].我国食品添加剂,2007,5:153-156.
[16]易建华,仇农学,胡冰,朱振宝.苹果浓缩汁中富马酸含量初步研究[J].我国果菜,2001,6:24
[17]阎晓莉,马维君,左荣.果汁中富马酸的来源、检测及控制[J].西北农林科技大学学报(自然科学版),2003,31(5):118-120.
[18]唐长波,岳田利.固相萃取分离苹果汁中富马酸的方法研究[J].食品研究与开发,2007,28(2):120-123.
[19]朱振宝,田呈瑞,易建华.影响苹果浓缩汁中富马酸因素的研究[J].饮料工业,2002,5(2):19-21.
[20]唐长波,岳田利.近红外光谱法检测果汁中的富马酸[J].西北农业学报,2007,16(2):187-189.
[21]高翠英,李彦威,梁改云.紫外分光光度法测定富马酸含量的新方法[J].分析试验室,2007,第26卷增刊:281-283.
[22]汤晓勤,向仕学,吕春燕.单扫描极谱法测定饮料果酒中富马酸[J].中华预防医学杂志,1999,33(4):239-240.
[23]C.Rivasseau,A.M.Boisson,G.Mongélard,G.Couram,O.Bastien,R.Bligny.Rapid analysis of organic acids in plant extracts by capillary electrophoresis with indirect UV detection: Directed metabolic analyses during metal stress[J].Journal of Chromatography A,2006,1129(2):283-290.
[24]T.J.Barden,M.Y.Croft,E.J.Murby,R.J.Wells.Gas chromatographic determination of organic acids from fruit juices by combined resin mediated methylation and extraction in supercritical carbon dioxide[J].Journal of Chromatography A,1997,785(1-2):251-261.
[25]施介华,徐秀珠.反相高效液相色谱法分离和测定富马酸[J].分析化学,2000,28(4):470-472.
[26]赵树法.苹果浓缩汁中5-HMF和还原糖含量变化及其与浓缩汁褐变关系研究[J].中国食物与营养,2007(1):40-42.
[27]V.Gōkmen,J.Acar.Simultaneous determination of 5-hydroxymethylfurfural and patulin in apple juice by reversed-phase liquid chromatography[J].Journal of Chromatography A,1999,847:69-74.
[28]李 良,孟淑洁,陈晓云.水果蔬菜及其制品中羟甲基糠醛测定的研究[J].辽宁农业科学,2002(4):12-14.
[29]梁俪恩.紫外分光光度法测定腹膜透析液中的降解产物5-羟甲基糠醛[J].广东药学院学报,2003,19(2):133-134.
[30]王丰,谢英新.HPLC法测定四物合剂中5-羟甲基糠醛的含量[J].黑龙江医药,2007,20(5):425-426.
[31]刘峰群,朱姗薇,赵庆国,韩晋,刘丽萍.棓丙酯葡萄糖注射液中5-羟甲基糠醛的HPLC 限量检查[J].我国药物应用与监测,2006(6):32-34.
[32]杨朝霞,李梅,董建军,武千钧.高效液相色谱同时测定啤酒中的5-羟甲基糠醛和糠醛[J].酿酒科技,2006(9):88-90.
[33]吴榕,孟瑾,韩奕奕.高效液相色谱法测定牛乳中的5-羟甲基糠醛[J].食品工业,2006(4):49-51.
[34]黄循明.HPLC检测长春西汀葡萄糖注射液中降解产物5-羟甲基糠醛[J].华西药学杂志,2005,20(6):546-547.
[35]朱振宝,易建华,寇晓康.苹果汁中展青霉素的吸附动力学研究[J].食品科学,2006,27(6):91-95.
[36]W.J.deKoe.Regulations in the EU on Mycotoxins in Foods[J].食品科学,2002,23(11):146-155.
[37]王云凤,常春艳,葛宝坤,王志英,黄国明.饮料中展青霉素和5-羟甲基糠醛的液相色谱-质谱测定方法[J].中国卫生检验杂志,2007,17(5):841-842.
[38]赵珊,李凤琴,陈丽娟,李玉伟,丁晓静,赵熙,吴多加,韩春卉,张宏元,计融.多功能柱净化-高效液相色谱法测定果汁中展青霉素[J].卫生研究,2007,36(5):634-636.
[39]殷居易,倪梅林,谢东华,李佐卿,房科腾,章再婷.高效液相色谱测定苹果浓缩汁展青霉素的残留量[J].分析科学学报,2007,23(1):119-121.
[40]李红光,陈艳,任磊.果汁中展青霉素的高效液相色谱测定法[J].职业与健康,2006,22(14):1076-1077.
[41]周克权,王君,刘秀梅.苹果汁中展青霉素和轻甲基糠醛的高效液相色谱测定方法[J].中国食品学报,2003,3(3):24-29.
[42]刘勇,胡文娟.苹果及其制品中展青霉素的薄层扫描测定法[J].卫生研究,1988,17(4):42-46.
[43]J.T.Edward,M.S.Peter.Determination of patulin by capillary gas chromatography of the heptafluorobutyrate derivative[J].Journal of chromatography A,1991,538(2):441-446.
[44]宋家玉,于国防,魏秀华,冷传祝,张建国,戚瑞玲.反相高效液相色谱法快速测定果汁 中展青霉素[J].中国卫生检验杂志,1999,9(3):227-228.
[45]H.Mhadhbi,S.Benrejeb,A.Martel.Studies on the affinity chromatography purification of anti-patulin polyclonal antibodies by enzyme linked immunosorbent assay and electrophoresis[J].Food additives and contaminants,2005,22(12):1243-1251.
[46]V.Sewram,J.J.Nair,T.W.Nieuwoudt,N.L.Leggott,G.S.Shephard.Determination of patulin in apple juice by high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry[J].Journal of Chromatography A,2000,897:365-374.
[47]R.Tsao,T.Zhou.Micellar electrokinetic capillary electrophoresis for rapid analysis of patulin in apple cider[J].Journal of Agricultural and Food Chemistry,2000,48:5231-5235.
[48]仲岳桐,柳其芳,罗若荣.高效液相色谱-质谱联用法检测果汁中的展青霉素[J].中国卫生检验杂志,2007,17(10):1778-1779.
[49]张艺兵,李寅宾,张鹏,赵卫东.高效液相色谱法测定苹果汁中的展青霉素[J].卫生研究,1998,第27卷增刊:146-148.
[50]R.Ito,H.Yamazaki,K.Inoue,Y.Yoshimura,M.Kawaguchi,H.Nakazawa.Development of liquid chromatography electrospray mass spectrometry for the determination of patulin in apple Juice:Investigation of Its contamination levels in Japan[J].Journal of Agricultural and Food Chemistry,2004,52:7464-7468.
[51]V.GOkmen,J.Acar,K.Sarioglu.Liquid chromatographic method for the determination of patulin in apple juice using solid-phase extraction[J].Analytica Chimica Acta,2005,543:64-69.
[52]V.Gokmen,J.Acar.Rapid reversed-phase liquid chromatographic determination of patulin in apple juice[J].Journal of Chromatography A,1996,730:53-58.
[53]J.K.Li,R.N.Wu,Q.H.Hu,J.H.Wang.Solid-phase extraction and HPLC determination of patulin in apple juice concentrate[J].Food Control,2007,18:530-534.
[54]黄永春.农药残留固化酶速测技术及应用研究[D].中国农业科学院,2003.
[55]江国虹,霍飞,李静,王荫国,曹慧丽.天津地区果蔬农药施用与残留状况及控制对策[J].中华预防医学杂志,2003,37(5):351-354.
[56]冯建国,陶训,于毅,张安盛.苹果园的污染和病虫无公害防治技术研究[J].中国果树,2000,2:9-13.
[57]聂继云,李静,李海飞,王孝娣.中国和国际组织规定的苹果中农药最大残留限量[J].落叶果树,2006,(1):16-17.
[58]杨振锋,马智勇.聂继云.联合国粮农组织对苹果农药最高残留量的规定[J].中国果树,2001,1:57.
[59]Y.Ito,T.Goto,S.Yamada,T.Ohno,H.Matsumoto,H.Oka,Y.lto.Rapid determination of carbamate pesticides in food using dual counter-current chromatography directly interfaced with mass spectrometry[J].Journal of Chromatography A,2008,1187(1-2):53-57.
[60]H.Y.Chiu,Z.Y.Lin,H.L.Tu,Ch.W.Whang.Analysis of glyphosate and aminomethylphosphonic acid by capillary electrophoresis with electrochemiluminescence detection[J].Journal of Chromatography A,2008,1177(1):195-198.
[61]I.Rezic,A.J.M.Horvat,S.Babic,M.K.Macan.Determination of pesticides in honey by ultrasonic solvent extraction and thin-layer chromatography[J].Ultrasonics Sonochemistry,2005,12(6):477-481.
[62]林子俺,龚巧燕,林旭聪.超声波提取-高效液相色谱测定茶叶中拟除虫菊酯农药残留[J].光谱实验室.2007.24(4):675-678.
[63]J.Cochran.Evaluation of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry for the determination of pesticides in tobacco 2008,1186:202-210.
[64]S.Walorczyk.Development of a multi-residue screening method for the determination of pesticides in cereals and dry animal feed using gas chromatography-triple quadrupole tandem mass spectrometry[J].Journal of Chromatography A,2007,1165(1-2):200-212.
[65]L.Mondello,A.Salvatore,P.Q.Tranchida,A.Casilli,P.Dugo,G.Dugo.Reliable identification of pesticides using linear retention indices as an active tool in gas chromatographic-mass spectrometric analysis[J].Journal of Chromatography A,2008,1186(1-2):430-433
[66]C.C.Leandro,P.Hancock,R.J.Fussell,B.J.Keely.Comparison of ultra-performance liquid chromatography and high-performance liquid chromatography for the determination of priority pesticides in baby foods by tandem quadrupole mass spectrometry[J].Journal of Chromatography A,2006,1103(1):94-101.
[67]M.H.Bernhard,L.Hofbauer,J.M(u|¨)ller.Method development for the determination of selected pesticides on tobacco by high-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry[J].Talanta,2008,74:1184-1190.
[68]Y.Pico,M.L.Farre,C.Soler,D.Barcel6.ldentification of unknown pesticides in fruits using ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry Imazalil as a case study of quantification[J].Journal of Chromatography A,2007,1176:123-134.
[69]张建春,胡筱青.红外光谱快速检验常见农药[J].广东公安科技,2006,3:31-33.
[70]S.Armenta,S.Garrigues,M.D.L.Guardia.Optimization of transmission near infrared spectrometry procedures for quality control of pesticide formulations[J].Analytica Chimica Acta,2006,571(2):288-297.
[71]L.Zhou,Z.Luo,S.M.Wang,Y.Hui,Z.D.Hu,X.G.Chen.In-capillary derivatization and laser-induced fluorescence detection for the analysis of organophosphorus pesticides by micellar electrokinetic chromatography[J].Journal of Chromatography A,2007,1149(2):377-384.
[72]Q.Zhang,Q.Sun,B.S.Hu,Q.Shen,G.Yang,X.Liang,X.Sun,F.Q.Liu.Development of a sensitive ELISA for the analysis of the organophosphorous insecticide fenthion in fruit sample[J].Food Chemistry,2008,106(3):1278-1284.
[73]W.Y.Lee,E.K.Lee,Y.J.Kim,W.C.Park,T.Chung,Y.T.Lee.Monoclonal antibody-based enzyme-linked immunosorbent assays for the detection of the organophosphorus insecticide isofenphos[J].Analytica Chimica Acta,2006,557(1-2):169-178.
[74]骆爱兰,余向阳,张存政,祝树德,刘贤进.拟除虫菊酯类农药多残留酶免疫分析方法的建立[J].中国农业科学,2005,38(2):308-312.
[75]朱国念,吴慧明,杨挺,吴刚,胡秀卿.利用放射免疫法测定水中克百威的研究[J].核农学报,2004,18(6):485-488.
[76]王战辉,张素霞,沈建忠,Sergei A E.荧光偏振免疫分析在农药和兽药残留检测中的研究进展[J].光谱学与光谱分析,2007,27(11):2299-2306.
[77]李方实,祝清兰.流动注射免疫分析及其在环境中农药残留分析研究综述[J].环境污染治理 技术与设备,2005,6(1):8-13.
[78]S.Suwansa-ard,P.Kanatharana,P.Asawatreratanakul,C.Limsakul,B.Wongkittisuksa,P.Thavarungkul.Semi disposable reactor biosensors for detecting carbamate pesticides in water[J].Biosensors and Bioelectronics,2005,21(3):445-454.
[79]F.Arduini,E Ricci,C.S.Tuta,D.Moscone,A.Amine,G.Pallesch.Detection of carbamic and organophosphorous pesticides in water samples using a cholinesterase biosensor based on Prussian Blue-modified screen-printed electrode[J].Analytica Chimica Acta,2006,580(2):155-162.
[80]S.Laschi,D.Ogonczyk,I.Palchetti,M.Mascini.Evaluation of pesticide-induced acetyleholinesterase inhibition by means of disposable carbon-modified electrochemical biosensors[J].Enzyme and Microbial Technology,2007,40(3):485-489.
[81]D.Du,X.Huang,J.Cai,A.Zhang.Amperometric detection of triazophos pesticide using acetylcholinesterase biosensor based on multiwall carbon nanotube-chitosan matdx[J].Sensors and Actuators B:Chemical,2007,127(2):531-535.
[82]D.Du,J.W.Ding,J.Cai,A.D.Zhang.Determination of carbaryl pesticide using amperometrie acetylcholinesterase sensor formed by electrochemically deposited chitosan[J].Colloids and Surfaces B:Biointerfaces,2007,58(2):145-150.
[83]H.Y.No,Y.A.Kim,Y.T.Lee,H.S.Lee.Cholinesterase-based dipstick assay for the detection of organophosphate and carbamate pesticides[J].A nalytica Chimica Acta,2007,594(1):37-43.
[84]杨娟,阮长青,闫美珍,孟祥宇.植物胆碱酯酶抑制法分析有机磷农药残留的研究[J].黑龙江八一农垦大学学报.2006.18(5):55-58.
[85]L.Campanella,A.Bonanni,E.Martini,N.Todini,M.Tomassetti.Determination of triazine pesticides using a new enzyme inhibition tyrosinase OPEE operating in chioroform[J].Sensors and Actuators B:Chemical,2005,111-112:505-514.
[86]胡贻椿,岳田利,袁亚宏,高振鹏.苹果浓缩汁生产环境中嗜酸耐热菌的分离与初步鉴定[J].西北农林科技大学学报(自然科学版),2007,35(5):184-188.
[87]胡贻椿,岳田利,袁亚宏,崔璐.苹果浓缩汁车间空气中嗜酸耐热菌的分离鉴定研究[J].农产品加工·学刊,2007,3:11-14.
[88]冯再平,仇农学,李建科.PCR法检测耐热菌模板制备方法研究[J].中兽医医药杂志,2006,4:5-6.
[89]关健,岳田利,薛淑静,袁亚宏,蔡福带.苹果汁中耐热菌培养基的优化及生长曲线[J].食品工业科技,2006,5:100-102.
[90]李建科,冯再平,仇农学.耐热菌的竞争定量PCR检测方法优化与建立[J].中国农业科学,2006,39(2):375-380.
[91]丁辰.果汁中嗜酸耐热菌的检测及控制[J].我国果菜,2006,2:39-40.
[92]薛晚利,周 玲,李选社,石兴民.苹果浓缩汁中嗜酸耐热菌的分离及检测条件探讨[J].西安交通大学学报(医学版),2005,26(2):199-200.
[93]王宏,常玉华,仇农学.PCR法检测耐热耐酸菌条件的优化[J].食品与发酵工业,2004,30(11):99-102.
[94]焦中高,土思新,段丛梅,刘杰超.苹果浓缩汁中耐热菌的分离及其生长特性的初步研究[J].食品科学,2003,24(9):85-87.
[95]蒋宏伟,张耀相,李高华,潘红延,魏守琦.苹果浓缩汁中耐热耐酸菌的检验[J].检验检疫 科学,2002,12(4):44-45.
[96]姚培鑫,马小魁.浓缩果汁生产厂中嗜酸耐热菌的跟踪检测[J].饮料工业,2001,4(3):42-45.
[97]王思新,焦中高,王晓燕.苹果浓缩汁加工中耐热菌的分析与控制[J].食品科学,2000,21(9):54-56.
[98]P.P.Vazquez,A.R.Mughari,M.M.Galera.Application of solid-phase microextraction for determination of pyrethroids in groundwater using liquid chromatography with post-column photochemieally induced fluorimetry derivatization and fluorescence detection[J].Journal of Chromatography A,2008,1188:61-68.
[99]徐明敏,陈波.变波长紫外液相色谱法测定果汁中5种人工合成色素[J].浙江预防医学,2007,19(5):93-94.
[100]张晓亮.高效液相色谱法测定果汁中的防腐剂和甜味剂的含量[J].检测与分析,2007,10(7):40-42.
[101]李永库,李晓静,欧小辉.果汁中9种酚酸类化合物的RP.HPLC-PAD分析[J].分析与检测,2007,33(7):135-138.
[102]王小莉,杨大进,李燕俊.高效液相色谱法测定果汁饮料中的糖精钠[J].中国热带医学,2005,5(7):1528-1529.
[103]胡志雄,张维农.HPLC-DAD测定果汁饮料中抗坏血酸总含量[J].武汉工业学院学报,2005,24(3):11-14.
[104]夏虹,杨沽,涂一名,蒙缔亚.离子对高效液相色谱法测定果汁中的合成色素[J].分析科学学报,2005,21(2):223-224.
[105]S.B.Consuelo,M.Esther,J.L.Tadeo.Determination of organochlorine pesticides in sewage sludge by matrix solid-phase dispersion and gas chromatography-mass spectrometry[J].Talanta,2008,74:1211-1217.
[106]许庆琴.大孔径毛细管气相色谱法测定野生果汁中的氨基酸[J].山西师范人学学报(自然科学版),2002,16(1):49-51.
[107]杨康,岳田利,袁亚宏,丰凡.利用顶空SPME-GC-MS联用技术检测苹果汁中嗜酸耐热菌代谢产物的研究[J].农产品加工.学刊,2007,3:8-11.
[108]C.Lesueur,M.Gartner,A.Mentler,M.Fuerhacker.Comparison of tour extraction methods for the analysis of 24 pesticides in soil samples with gas chromatography-mass spectrometry and liquid chromatography-ion trap-mass spectrometry[J].Talanta,2008,75:284-293.
[109]高海燕,廖小军,王善广,胡小松.反相高效液相色谱法测定果汁中11种有机酸条件的优化[J].分析化学,2004,32(12):1645-1648.
[110]M.H.lha,M.Sabino.Incidence of patulin in Brazilian apple-based drinks[J].Food Control,2008,19:417-422.
[111]H.Morales,V.Sanchis,A.Rovira,A.J.Ramos,S,Matin.Patulin accumulation in apples during postharvest:effect of controlled atmosphere storage and fungicide treatments[J].Food Control,2007,18:1443-1448.
[112]S.Drusch,S.Kopka,J.Kaeding.Stability of patulin in a juice-like aqueous model system in the presence of ascorbic acid[J].Food Chemistry,2007,100(l):192-197.
[113]刘晓松,高欣,重张法,刘军义.固相萃取-HPLC法测定浓缩梨汁中噻菌灵、多菌灵的残留量[J].分析测试技术与仪器,2006,12(3):131-135.
[114]吴伟都,金世梅,朱慧.自动进样顶空气相色谱法测定浓缩果汁中的乙醇[J].中国食品添 加剂,2004,5:97-99.
[115]张艺兵,鲍蕾,楮庆华.农产品中真菌毒素的检测分析[M],化学工业出版社,2006:234
[116]GB9558-2001,晶体乐果[S].
[117]罗安才,杨晓红,邓英毅,李纯凡,向可术,李道高.柑橘果实发育过程中有机酸含量及相关代谢酶活性的变化[J].中国农业科学,2003,36(8):941-944.
[118]郑仲,何品晶,邵立明.沥滤液中低分子量有机酸对小麦种子的急性毒性[J].农业环境科学学报,2006,25(5):1138-1142.
[119]D.Bylund,S.H.Norstr(o|¨)m,S.A.Essen,U.S.Lundstr(o|¨)m.Analysis of low molecular mass organic acids in natural waters by ion exclusion chromatography tandem mass spectrometry[J].Journal of Chromatography A,2007,1176(1-2):89-93.
[120]C.I.Rodrigues,L.Marta,R.Maia,M.Miranda,M.Ribeidnho,C.Maguas.Application of solid-phase extraction to brewed coffee caffeine and organic acid determination by UV/HPLC[J].Journal of Food Composition and Analysis,2007,20(5):440-448.
[121]周克权,王君,刘秀梅.苹果汁中展青霉素和羟甲基糠醛的高效液相色谱测定方法[J].中国食品学报,2003,3(3):24-29.
[122]S.G.Shephard,N.L.Leggott.Chromatographic determination of the mycotoxin patulin in fruit and fruit juices[J].Journal of Chromatography A,2000,882:17-22.
[123]周俊,乔坤云,冯婷,孙晓陆.番茄酱、果汁及果酒中展青霉素的检测与分析[J].现代科学仪器,2006,1:113-114.
[124]乌日娜.苹果及其浓缩汁中展青霉素和主要有机磷农药的残留分析研究[D].陕西师范大学硕士学位论文.2005.
[2]白志礼,穆养民,赵政阳.陕西苹果产业发展的新思考与新探索[J].干旱地区农业研究,2003,21(4):172-175.
[3]赵政阳,冯宝荣,王雷存,王章陵,周卫国.我国苹果产业向优势区域集中的战略思考[J].西北农业学报,2004,13(4):195-199.
[4]赵贵宝.我国苹果浓缩汁加工出口的形势、问题与对策[J].陕西农业科学,2004,5:63-66.
[5]张敬滋.我国小苹果做出世界大文章-中国苹果浓缩汁行业发展概况综述[J].农村实用工程技术.农业产业化,2004,2:35-38.
[6]仇农学,肖旭霖,邓红.陕西省苹果浓缩汁行业可持续发展的战略思考[J].农业工程学报,2000,16(1):122-124.
[7]成喜玲.陕西苹果汁加工业存在的问题及其对策[J].陕西省行政学院.陕西省经济管理干部学院学报,2005,19(2):43-46.
[8]解维域.苹果浓缩汁中若干重要质量指标的检测与控制[J].我国果菜,2001,3:25.
[9]柳畅先,庹浔,吴士筠.酶法测定乳酸[J].分析试验室,2005,24(9):75-77.
[10]V.Galli,C.Barbas.Capillary electrophoresis for the analysis of short-chain organic acids in coffee[J].Journal of Chromatography A,2004,1032(1-2) 1:299-304.
[11]王俊华,杨洁,申彤.乳酸发酵胡萝卜汁中有机酸的HPLC测定[J].现代食品科技,2006,4:235-238.
[12]章新,朱惠贤,王林,杨光宇,胡秋芬.用快速分离柱高效液相色谱法测定生物发酵产物中的乳酸[J].我国酿造,2005,7:53-54.
[13]汤丽芬,吴珏珩,张选红,陈健文,陈红英,林广云.高效液相色谱法同时测定小鼠脑组织中乳酸与磷酸肌酸含量[J].中国卫生检验杂志,2005,15(3):300-302.
[14]朱振宝,田呈瑞,易建华,朱粉莉.苹果汁中富马酸的吸附[J].陕西科技大学学报,2001,21(3):36-39.
[15]陈爱华,焦必宁.常见果汁掺假检测技术的研究进展[J].我国食品添加剂,2007,5:153-156.
[16]易建华,仇农学,胡冰,朱振宝.苹果浓缩汁中富马酸含量初步研究[J].我国果菜,2001,6:24
[17]阎晓莉,马维君,左荣.果汁中富马酸的来源、检测及控制[J].西北农林科技大学学报(自然科学版),2003,31(5):118-120.
[18]唐长波,岳田利.固相萃取分离苹果汁中富马酸的方法研究[J].食品研究与开发,2007,28(2):120-123.
[19]朱振宝,田呈瑞,易建华.影响苹果浓缩汁中富马酸因素的研究[J].饮料工业,2002,5(2):19-21.
[20]唐长波,岳田利.近红外光谱法检测果汁中的富马酸[J].西北农业学报,2007,16(2):187-189.
[21]高翠英,李彦威,梁改云.紫外分光光度法测定富马酸含量的新方法[J].分析试验室,2007,第26卷增刊:281-283.
[22]汤晓勤,向仕学,吕春燕.单扫描极谱法测定饮料果酒中富马酸[J].中华预防医学杂志,1999,33(4):239-240.
[23]C.Rivasseau,A.M.Boisson,G.Mongélard,G.Couram,O.Bastien,R.Bligny.Rapid analysis of organic acids in plant extracts by capillary electrophoresis with indirect UV detection: Directed metabolic analyses during metal stress[J].Journal of Chromatography A,2006,1129(2):283-290.
[24]T.J.Barden,M.Y.Croft,E.J.Murby,R.J.Wells.Gas chromatographic determination of organic acids from fruit juices by combined resin mediated methylation and extraction in supercritical carbon dioxide[J].Journal of Chromatography A,1997,785(1-2):251-261.
[25]施介华,徐秀珠.反相高效液相色谱法分离和测定富马酸[J].分析化学,2000,28(4):470-472.
[26]赵树法.苹果浓缩汁中5-HMF和还原糖含量变化及其与浓缩汁褐变关系研究[J].中国食物与营养,2007(1):40-42.
[27]V.Gōkmen,J.Acar.Simultaneous determination of 5-hydroxymethylfurfural and patulin in apple juice by reversed-phase liquid chromatography[J].Journal of Chromatography A,1999,847:69-74.
[28]李 良,孟淑洁,陈晓云.水果蔬菜及其制品中羟甲基糠醛测定的研究[J].辽宁农业科学,2002(4):12-14.
[29]梁俪恩.紫外分光光度法测定腹膜透析液中的降解产物5-羟甲基糠醛[J].广东药学院学报,2003,19(2):133-134.
[30]王丰,谢英新.HPLC法测定四物合剂中5-羟甲基糠醛的含量[J].黑龙江医药,2007,20(5):425-426.
[31]刘峰群,朱姗薇,赵庆国,韩晋,刘丽萍.棓丙酯葡萄糖注射液中5-羟甲基糠醛的HPLC 限量检查[J].我国药物应用与监测,2006(6):32-34.
[32]杨朝霞,李梅,董建军,武千钧.高效液相色谱同时测定啤酒中的5-羟甲基糠醛和糠醛[J].酿酒科技,2006(9):88-90.
[33]吴榕,孟瑾,韩奕奕.高效液相色谱法测定牛乳中的5-羟甲基糠醛[J].食品工业,2006(4):49-51.
[34]黄循明.HPLC检测长春西汀葡萄糖注射液中降解产物5-羟甲基糠醛[J].华西药学杂志,2005,20(6):546-547.
[35]朱振宝,易建华,寇晓康.苹果汁中展青霉素的吸附动力学研究[J].食品科学,2006,27(6):91-95.
[36]W.J.deKoe.Regulations in the EU on Mycotoxins in Foods[J].食品科学,2002,23(11):146-155.
[37]王云凤,常春艳,葛宝坤,王志英,黄国明.饮料中展青霉素和5-羟甲基糠醛的液相色谱-质谱测定方法[J].中国卫生检验杂志,2007,17(5):841-842.
[38]赵珊,李凤琴,陈丽娟,李玉伟,丁晓静,赵熙,吴多加,韩春卉,张宏元,计融.多功能柱净化-高效液相色谱法测定果汁中展青霉素[J].卫生研究,2007,36(5):634-636.
[39]殷居易,倪梅林,谢东华,李佐卿,房科腾,章再婷.高效液相色谱测定苹果浓缩汁展青霉素的残留量[J].分析科学学报,2007,23(1):119-121.
[40]李红光,陈艳,任磊.果汁中展青霉素的高效液相色谱测定法[J].职业与健康,2006,22(14):1076-1077.
[41]周克权,王君,刘秀梅.苹果汁中展青霉素和轻甲基糠醛的高效液相色谱测定方法[J].中国食品学报,2003,3(3):24-29.
[42]刘勇,胡文娟.苹果及其制品中展青霉素的薄层扫描测定法[J].卫生研究,1988,17(4):42-46.
[43]J.T.Edward,M.S.Peter.Determination of patulin by capillary gas chromatography of the heptafluorobutyrate derivative[J].Journal of chromatography A,1991,538(2):441-446.
[44]宋家玉,于国防,魏秀华,冷传祝,张建国,戚瑞玲.反相高效液相色谱法快速测定果汁 中展青霉素[J].中国卫生检验杂志,1999,9(3):227-228.
[45]H.Mhadhbi,S.Benrejeb,A.Martel.Studies on the affinity chromatography purification of anti-patulin polyclonal antibodies by enzyme linked immunosorbent assay and electrophoresis[J].Food additives and contaminants,2005,22(12):1243-1251.
[46]V.Sewram,J.J.Nair,T.W.Nieuwoudt,N.L.Leggott,G.S.Shephard.Determination of patulin in apple juice by high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry[J].Journal of Chromatography A,2000,897:365-374.
[47]R.Tsao,T.Zhou.Micellar electrokinetic capillary electrophoresis for rapid analysis of patulin in apple cider[J].Journal of Agricultural and Food Chemistry,2000,48:5231-5235.
[48]仲岳桐,柳其芳,罗若荣.高效液相色谱-质谱联用法检测果汁中的展青霉素[J].中国卫生检验杂志,2007,17(10):1778-1779.
[49]张艺兵,李寅宾,张鹏,赵卫东.高效液相色谱法测定苹果汁中的展青霉素[J].卫生研究,1998,第27卷增刊:146-148.
[50]R.Ito,H.Yamazaki,K.Inoue,Y.Yoshimura,M.Kawaguchi,H.Nakazawa.Development of liquid chromatography electrospray mass spectrometry for the determination of patulin in apple Juice:Investigation of Its contamination levels in Japan[J].Journal of Agricultural and Food Chemistry,2004,52:7464-7468.
[51]V.GOkmen,J.Acar,K.Sarioglu.Liquid chromatographic method for the determination of patulin in apple juice using solid-phase extraction[J].Analytica Chimica Acta,2005,543:64-69.
[52]V.Gokmen,J.Acar.Rapid reversed-phase liquid chromatographic determination of patulin in apple juice[J].Journal of Chromatography A,1996,730:53-58.
[53]J.K.Li,R.N.Wu,Q.H.Hu,J.H.Wang.Solid-phase extraction and HPLC determination of patulin in apple juice concentrate[J].Food Control,2007,18:530-534.
[54]黄永春.农药残留固化酶速测技术及应用研究[D].中国农业科学院,2003.
[55]江国虹,霍飞,李静,王荫国,曹慧丽.天津地区果蔬农药施用与残留状况及控制对策[J].中华预防医学杂志,2003,37(5):351-354.
[56]冯建国,陶训,于毅,张安盛.苹果园的污染和病虫无公害防治技术研究[J].中国果树,2000,2:9-13.
[57]聂继云,李静,李海飞,王孝娣.中国和国际组织规定的苹果中农药最大残留限量[J].落叶果树,2006,(1):16-17.
[58]杨振锋,马智勇.聂继云.联合国粮农组织对苹果农药最高残留量的规定[J].中国果树,2001,1:57.
[59]Y.Ito,T.Goto,S.Yamada,T.Ohno,H.Matsumoto,H.Oka,Y.lto.Rapid determination of carbamate pesticides in food using dual counter-current chromatography directly interfaced with mass spectrometry[J].Journal of Chromatography A,2008,1187(1-2):53-57.
[60]H.Y.Chiu,Z.Y.Lin,H.L.Tu,Ch.W.Whang.Analysis of glyphosate and aminomethylphosphonic acid by capillary electrophoresis with electrochemiluminescence detection[J].Journal of Chromatography A,2008,1177(1):195-198.
[61]I.Rezic,A.J.M.Horvat,S.Babic,M.K.Macan.Determination of pesticides in honey by ultrasonic solvent extraction and thin-layer chromatography[J].Ultrasonics Sonochemistry,2005,12(6):477-481.
[62]林子俺,龚巧燕,林旭聪.超声波提取-高效液相色谱测定茶叶中拟除虫菊酯农药残留[J].光谱实验室.2007.24(4):675-678.
[63]J.Cochran.Evaluation of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry for the determination of pesticides in tobacco 2008,1186:202-210.
[64]S.Walorczyk.Development of a multi-residue screening method for the determination of pesticides in cereals and dry animal feed using gas chromatography-triple quadrupole tandem mass spectrometry[J].Journal of Chromatography A,2007,1165(1-2):200-212.
[65]L.Mondello,A.Salvatore,P.Q.Tranchida,A.Casilli,P.Dugo,G.Dugo.Reliable identification of pesticides using linear retention indices as an active tool in gas chromatographic-mass spectrometric analysis[J].Journal of Chromatography A,2008,1186(1-2):430-433
[66]C.C.Leandro,P.Hancock,R.J.Fussell,B.J.Keely.Comparison of ultra-performance liquid chromatography and high-performance liquid chromatography for the determination of priority pesticides in baby foods by tandem quadrupole mass spectrometry[J].Journal of Chromatography A,2006,1103(1):94-101.
[67]M.H.Bernhard,L.Hofbauer,J.M(u|¨)ller.Method development for the determination of selected pesticides on tobacco by high-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry[J].Talanta,2008,74:1184-1190.
[68]Y.Pico,M.L.Farre,C.Soler,D.Barcel6.ldentification of unknown pesticides in fruits using ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry Imazalil as a case study of quantification[J].Journal of Chromatography A,2007,1176:123-134.
[69]张建春,胡筱青.红外光谱快速检验常见农药[J].广东公安科技,2006,3:31-33.
[70]S.Armenta,S.Garrigues,M.D.L.Guardia.Optimization of transmission near infrared spectrometry procedures for quality control of pesticide formulations[J].Analytica Chimica Acta,2006,571(2):288-297.
[71]L.Zhou,Z.Luo,S.M.Wang,Y.Hui,Z.D.Hu,X.G.Chen.In-capillary derivatization and laser-induced fluorescence detection for the analysis of organophosphorus pesticides by micellar electrokinetic chromatography[J].Journal of Chromatography A,2007,1149(2):377-384.
[72]Q.Zhang,Q.Sun,B.S.Hu,Q.Shen,G.Yang,X.Liang,X.Sun,F.Q.Liu.Development of a sensitive ELISA for the analysis of the organophosphorous insecticide fenthion in fruit sample[J].Food Chemistry,2008,106(3):1278-1284.
[73]W.Y.Lee,E.K.Lee,Y.J.Kim,W.C.Park,T.Chung,Y.T.Lee.Monoclonal antibody-based enzyme-linked immunosorbent assays for the detection of the organophosphorus insecticide isofenphos[J].Analytica Chimica Acta,2006,557(1-2):169-178.
[74]骆爱兰,余向阳,张存政,祝树德,刘贤进.拟除虫菊酯类农药多残留酶免疫分析方法的建立[J].中国农业科学,2005,38(2):308-312.
[75]朱国念,吴慧明,杨挺,吴刚,胡秀卿.利用放射免疫法测定水中克百威的研究[J].核农学报,2004,18(6):485-488.
[76]王战辉,张素霞,沈建忠,Sergei A E.荧光偏振免疫分析在农药和兽药残留检测中的研究进展[J].光谱学与光谱分析,2007,27(11):2299-2306.
[77]李方实,祝清兰.流动注射免疫分析及其在环境中农药残留分析研究综述[J].环境污染治理 技术与设备,2005,6(1):8-13.
[78]S.Suwansa-ard,P.Kanatharana,P.Asawatreratanakul,C.Limsakul,B.Wongkittisuksa,P.Thavarungkul.Semi disposable reactor biosensors for detecting carbamate pesticides in water[J].Biosensors and Bioelectronics,2005,21(3):445-454.
[79]F.Arduini,E Ricci,C.S.Tuta,D.Moscone,A.Amine,G.Pallesch.Detection of carbamic and organophosphorous pesticides in water samples using a cholinesterase biosensor based on Prussian Blue-modified screen-printed electrode[J].Analytica Chimica Acta,2006,580(2):155-162.
[80]S.Laschi,D.Ogonczyk,I.Palchetti,M.Mascini.Evaluation of pesticide-induced acetyleholinesterase inhibition by means of disposable carbon-modified electrochemical biosensors[J].Enzyme and Microbial Technology,2007,40(3):485-489.
[81]D.Du,X.Huang,J.Cai,A.Zhang.Amperometric detection of triazophos pesticide using acetylcholinesterase biosensor based on multiwall carbon nanotube-chitosan matdx[J].Sensors and Actuators B:Chemical,2007,127(2):531-535.
[82]D.Du,J.W.Ding,J.Cai,A.D.Zhang.Determination of carbaryl pesticide using amperometrie acetylcholinesterase sensor formed by electrochemically deposited chitosan[J].Colloids and Surfaces B:Biointerfaces,2007,58(2):145-150.
[83]H.Y.No,Y.A.Kim,Y.T.Lee,H.S.Lee.Cholinesterase-based dipstick assay for the detection of organophosphate and carbamate pesticides[J].A nalytica Chimica Acta,2007,594(1):37-43.
[84]杨娟,阮长青,闫美珍,孟祥宇.植物胆碱酯酶抑制法分析有机磷农药残留的研究[J].黑龙江八一农垦大学学报.2006.18(5):55-58.
[85]L.Campanella,A.Bonanni,E.Martini,N.Todini,M.Tomassetti.Determination of triazine pesticides using a new enzyme inhibition tyrosinase OPEE operating in chioroform[J].Sensors and Actuators B:Chemical,2005,111-112:505-514.
[86]胡贻椿,岳田利,袁亚宏,高振鹏.苹果浓缩汁生产环境中嗜酸耐热菌的分离与初步鉴定[J].西北农林科技大学学报(自然科学版),2007,35(5):184-188.
[87]胡贻椿,岳田利,袁亚宏,崔璐.苹果浓缩汁车间空气中嗜酸耐热菌的分离鉴定研究[J].农产品加工·学刊,2007,3:11-14.
[88]冯再平,仇农学,李建科.PCR法检测耐热菌模板制备方法研究[J].中兽医医药杂志,2006,4:5-6.
[89]关健,岳田利,薛淑静,袁亚宏,蔡福带.苹果汁中耐热菌培养基的优化及生长曲线[J].食品工业科技,2006,5:100-102.
[90]李建科,冯再平,仇农学.耐热菌的竞争定量PCR检测方法优化与建立[J].中国农业科学,2006,39(2):375-380.
[91]丁辰.果汁中嗜酸耐热菌的检测及控制[J].我国果菜,2006,2:39-40.
[92]薛晚利,周 玲,李选社,石兴民.苹果浓缩汁中嗜酸耐热菌的分离及检测条件探讨[J].西安交通大学学报(医学版),2005,26(2):199-200.
[93]王宏,常玉华,仇农学.PCR法检测耐热耐酸菌条件的优化[J].食品与发酵工业,2004,30(11):99-102.
[94]焦中高,土思新,段丛梅,刘杰超.苹果浓缩汁中耐热菌的分离及其生长特性的初步研究[J].食品科学,2003,24(9):85-87.
[95]蒋宏伟,张耀相,李高华,潘红延,魏守琦.苹果浓缩汁中耐热耐酸菌的检验[J].检验检疫 科学,2002,12(4):44-45.
[96]姚培鑫,马小魁.浓缩果汁生产厂中嗜酸耐热菌的跟踪检测[J].饮料工业,2001,4(3):42-45.
[97]王思新,焦中高,王晓燕.苹果浓缩汁加工中耐热菌的分析与控制[J].食品科学,2000,21(9):54-56.
[98]P.P.Vazquez,A.R.Mughari,M.M.Galera.Application of solid-phase microextraction for determination of pyrethroids in groundwater using liquid chromatography with post-column photochemieally induced fluorimetry derivatization and fluorescence detection[J].Journal of Chromatography A,2008,1188:61-68.
[99]徐明敏,陈波.变波长紫外液相色谱法测定果汁中5种人工合成色素[J].浙江预防医学,2007,19(5):93-94.
[100]张晓亮.高效液相色谱法测定果汁中的防腐剂和甜味剂的含量[J].检测与分析,2007,10(7):40-42.
[101]李永库,李晓静,欧小辉.果汁中9种酚酸类化合物的RP.HPLC-PAD分析[J].分析与检测,2007,33(7):135-138.
[102]王小莉,杨大进,李燕俊.高效液相色谱法测定果汁饮料中的糖精钠[J].中国热带医学,2005,5(7):1528-1529.
[103]胡志雄,张维农.HPLC-DAD测定果汁饮料中抗坏血酸总含量[J].武汉工业学院学报,2005,24(3):11-14.
[104]夏虹,杨沽,涂一名,蒙缔亚.离子对高效液相色谱法测定果汁中的合成色素[J].分析科学学报,2005,21(2):223-224.
[105]S.B.Consuelo,M.Esther,J.L.Tadeo.Determination of organochlorine pesticides in sewage sludge by matrix solid-phase dispersion and gas chromatography-mass spectrometry[J].Talanta,2008,74:1211-1217.
[106]许庆琴.大孔径毛细管气相色谱法测定野生果汁中的氨基酸[J].山西师范人学学报(自然科学版),2002,16(1):49-51.
[107]杨康,岳田利,袁亚宏,丰凡.利用顶空SPME-GC-MS联用技术检测苹果汁中嗜酸耐热菌代谢产物的研究[J].农产品加工.学刊,2007,3:8-11.
[108]C.Lesueur,M.Gartner,A.Mentler,M.Fuerhacker.Comparison of tour extraction methods for the analysis of 24 pesticides in soil samples with gas chromatography-mass spectrometry and liquid chromatography-ion trap-mass spectrometry[J].Talanta,2008,75:284-293.
[109]高海燕,廖小军,王善广,胡小松.反相高效液相色谱法测定果汁中11种有机酸条件的优化[J].分析化学,2004,32(12):1645-1648.
[110]M.H.lha,M.Sabino.Incidence of patulin in Brazilian apple-based drinks[J].Food Control,2008,19:417-422.
[111]H.Morales,V.Sanchis,A.Rovira,A.J.Ramos,S,Matin.Patulin accumulation in apples during postharvest:effect of controlled atmosphere storage and fungicide treatments[J].Food Control,2007,18:1443-1448.
[112]S.Drusch,S.Kopka,J.Kaeding.Stability of patulin in a juice-like aqueous model system in the presence of ascorbic acid[J].Food Chemistry,2007,100(l):192-197.
[113]刘晓松,高欣,重张法,刘军义.固相萃取-HPLC法测定浓缩梨汁中噻菌灵、多菌灵的残留量[J].分析测试技术与仪器,2006,12(3):131-135.
[114]吴伟都,金世梅,朱慧.自动进样顶空气相色谱法测定浓缩果汁中的乙醇[J].中国食品添 加剂,2004,5:97-99.
[115]张艺兵,鲍蕾,楮庆华.农产品中真菌毒素的检测分析[M],化学工业出版社,2006:234
[116]GB9558-2001,晶体乐果[S].
[117]罗安才,杨晓红,邓英毅,李纯凡,向可术,李道高.柑橘果实发育过程中有机酸含量及相关代谢酶活性的变化[J].中国农业科学,2003,36(8):941-944.
[118]郑仲,何品晶,邵立明.沥滤液中低分子量有机酸对小麦种子的急性毒性[J].农业环境科学学报,2006,25(5):1138-1142.
[119]D.Bylund,S.H.Norstr(o|¨)m,S.A.Essen,U.S.Lundstr(o|¨)m.Analysis of low molecular mass organic acids in natural waters by ion exclusion chromatography tandem mass spectrometry[J].Journal of Chromatography A,2007,1176(1-2):89-93.
[120]C.I.Rodrigues,L.Marta,R.Maia,M.Miranda,M.Ribeidnho,C.Maguas.Application of solid-phase extraction to brewed coffee caffeine and organic acid determination by UV/HPLC[J].Journal of Food Composition and Analysis,2007,20(5):440-448.
[121]周克权,王君,刘秀梅.苹果汁中展青霉素和羟甲基糠醛的高效液相色谱测定方法[J].中国食品学报,2003,3(3):24-29.
[122]S.G.Shephard,N.L.Leggott.Chromatographic determination of the mycotoxin patulin in fruit and fruit juices[J].Journal of Chromatography A,2000,882:17-22.
[123]周俊,乔坤云,冯婷,孙晓陆.番茄酱、果汁及果酒中展青霉素的检测与分析[J].现代科学仪器,2006,1:113-114.
[124]乌日娜.苹果及其浓缩汁中展青霉素和主要有机磷农药的残留分析研究[D].陕西师范大学硕士学位论文.2005.