QuEChERS提取方法結(jié)合超高效液相色譜串聯(lián)質(zhì)譜測(cè)定水、土和水稻中的氯代水楊胺
發(fā)布時(shí)間:2021-11-05 12:34
本研究采用Qu ECh ERS前處理方法,建立了一種利用超高效液相色譜-串聯(lián)質(zhì)譜(UPLC-MS/MS)檢測(cè)水、水稻和土壤中氯代水楊胺(LDS)的靈敏、快速、簡(jiǎn)便的殘留分析方法。氯代水楊胺(LDS)采用乙腈提取,Florisil和C18凈化。采用電噴霧離子源負(fù)離子電離模式,目標(biāo)化合物在3分鐘內(nèi)完成檢測(cè)。氯代水楊胺在水、水稻和土壤三種基質(zhì)中的平均回收率為82.54%99.9%,相對(duì)標(biāo)準(zhǔn)偏差為1.51%4.86%(n=5)。檢出限(LOD)小于0.011μg kg-1,定量限(LOQ)低于5μg kg-1,明顯低于澳大利亞制定的最大殘留限量。該方法簡(jiǎn)便可靠,滿足對(duì)水、水稻和土壤樣品中氯代水楊胺(LDS)的檢測(cè)。本研究為中國(guó)制定氯代水楊胺(LDS)在不同農(nóng)產(chǎn)品和環(huán)境樣品中的最大殘留水平和分析方法提供了理論基礎(chǔ)。
【文章來(lái)源】:中國(guó)農(nóng)業(yè)科學(xué)院北京市
【文章頁(yè)數(shù)】:60 頁(yè)
【學(xué)位級(jí)別】:碩士
【文章目錄】:
摘要
abstract
List of Abbreviations
CHAPTER 1 GEN ERAL IN TRO DUC TION
1.1 INTRODUCTION TO PESTICIDES
1.2 ORIGIN OF PESTICIDES
1.3 CLASSIFICATION OF PESTICIDES
1.3.1 Insecticides
1.3.2 Fungicides
1.3.3 Her bici des
1.3.4 Mi ticides
1.3.5 Rodenticides
1.3.6 Molluscicides
1.4 FORMULATION OF PESTICIDES
1.5 IMPACT OF PESTICIDES
1.5.1 Use in agriculture
1.5.2 Use in public and li vestock health
1.5.3 Other uses
1.6 RISK OF PESTICIDES USE IN THE ENVIRONMENT AND PUBLIC HEALTH
1.7 PESTICIDE RESIDUE
1.8 MAXIMUM RESIDUE LEVEL (MRLS) OF PESTICIDE
1.9 PESTICIDE RESIDUE ANALYSIS-AN OVERVIEW
1.10 SAMPLE PREPARATION TECHNIQUES
1.10.1 Quick, Easy, Che ap, Effec ti ve, Rugged, and Safe (Qu ECh ERS) extrac tion method
1.11 CHROMATOGRAPHIC SEPARATION TECHNIQUES
1.11.1 Gas chromatography (GC)
1.11.2 Li qui d chr omatogr aphy (LC)
1.12 DETERMINATION TECHNIQUES
1.12.1 Li qui d chr omatogr aphy couple d with tande m mass spectrometr y (LC -MS/ MS)
1.13 MATRIX PROBLEMS IN PESTICIDE RESIDUE ANALYSIS
1.14 CALIBRATION TECHNIQUES
1.15 TARGET PESTICIDES AND PROBLEM ASSOCIATED WITH THIS STUDY
1.16 AIMS AND OBJECTIVES OF THE STUDY
CHAPTER 2 DEVELOPMENT OF Qu ECh ERS BASED EXTRACTION METHOD FOR UPLC-MS/MS DETERMINATION OF QUINOID NICLOSAMIDE (LDS) RESIDUE IN WATER, SOIL AND RIC E SAMPLES
2.1 INTRODUCTION
2.2 MATERIALS AND METHODS
2.2.1 Che micals and re agents
2.2.2 Appar atus for sample pre paration
2.2.3 Chromatogr aphic and mass spectrometr y c ondi tion
2.2.4 Sample pre paration
2.2.5 Method vali dation
2.3 RESULTS AND DISCUSSION
2.3.1 Opti mization of instrumental c ondi tions
2.3.2 Opti mization of LC mobile phase solve nts
2.3.3 Opti mization of c hromatographic c ondi tion
2.3.4 Opti mization of the e xtracti on and cle anup pr oce dure
2.4 VALIDATION OF THE METHOD
2.4.1 The Li nearity
2.4.2 Accurac y and precision
2.4.3 Li mits of de tection (LOD) and quanti ficati on (LOQ)
2.4.4 Matrix e ffect
2.4.5 Application to re al samples
Chapter 3 CONCLUSION
References
Acknowledgement
Resume
【參考文獻(xiàn)】:
期刊論文
[1]QuEChERS/液相色譜串聯(lián)質(zhì)譜法測(cè)定水產(chǎn)品中氯硝柳胺[J]. 劉伶俐,萬(wàn)譯文,伍遠(yuǎn)安,索紋紋,肖維. 食品工業(yè)科技. 2016(23)
[2]高效液相色譜-質(zhì)譜/質(zhì)譜聯(lián)用法檢測(cè)漁業(yè)水體中氯硝柳胺[J]. 萬(wàn)譯文,黃向榮,李小玲,陳湘藝,黃華偉. 分析試驗(yàn)室. 2015(01)
[3]氯代水楊胺對(duì)山丘釘螺實(shí)驗(yàn)室和現(xiàn)場(chǎng)殺螺效果研究[J]. 張劍鋒,朱明東,嚴(yán)曉嵐,蔣能明,林麗君,黃禮蘭,俞麗玲,葉曉東,聞禮永. 中國(guó)媒介生物學(xué)及控制雜志. 2014(01)
[4]雙水相浮選-HPLC法測(cè)定水中氯硝柳胺[J]. 傅海珍,謝菊,陳晶晶,楊曉雙,侯健,戚雪勇. 環(huán)境科學(xué)與技術(shù). 2013(09)
[5]10%氯代水楊胺可濕性粉劑現(xiàn)場(chǎng)滅螺效果觀察[J]. 張瑕,張華明,劉雄,榮先斌,楊蕊. 中國(guó)血吸蟲(chóng)病防治雜志. 2013(02)
[6]殺螺胺乙醇胺鹽在水稻和稻田中的殘留及消解動(dòng)態(tài)[J]. 伍一紅,龔道新,張素芳,周圣超. 農(nóng)業(yè)環(huán)境科學(xué)學(xué)報(bào). 2012(02)
[7]超聲萃取-高效液相色譜測(cè)定土壤中的氯硝柳胺[J]. 周穎,周藝彪,何明禎,王海銀,屈衛(wèi)東,姜慶五. 中國(guó)血吸蟲(chóng)病防治雜志. 2009(01)
[8]新型滅螺劑氯代水楊胺滅螺效果研究[J]. 徐興建,元藝,李桂玲,魏鳳華,趙云斌,涂祖武,劉敏,曹慕民,何匯,范宏萍. 中國(guó)血吸蟲(chóng)病防治雜志. 2007(05)
[9]不同樣品的氯硝柳胺乙醇膠鹽可濕性粉劑的殺螺效果與質(zhì)量比較[J]. 戴建榮,陳昌,梁幼生,張燕萍,鄭育賢,房文. 中國(guó)血吸蟲(chóng)病防治雜志. 1998(02)
[10]氯硝柳胺對(duì)魚(yú)類和溞類的毒性研究[J]. 修瑞琴,陳昌,許永香,高世榮,任改英,鄭靜. 中國(guó)血吸蟲(chóng)病防治雜志. 1996(06)
本文編號(hào):3477806
【文章來(lái)源】:中國(guó)農(nóng)業(yè)科學(xué)院北京市
【文章頁(yè)數(shù)】:60 頁(yè)
【學(xué)位級(jí)別】:碩士
【文章目錄】:
摘要
abstract
List of Abbreviations
CHAPTER 1 GEN ERAL IN TRO DUC TION
1.1 INTRODUCTION TO PESTICIDES
1.2 ORIGIN OF PESTICIDES
1.3 CLASSIFICATION OF PESTICIDES
1.3.1 Insecticides
1.3.2 Fungicides
1.3.3 Her bici des
1.3.4 Mi ticides
1.3.5 Rodenticides
1.3.6 Molluscicides
1.4 FORMULATION OF PESTICIDES
1.5 IMPACT OF PESTICIDES
1.5.1 Use in agriculture
1.5.2 Use in public and li vestock health
1.5.3 Other uses
1.6 RISK OF PESTICIDES USE IN THE ENVIRONMENT AND PUBLIC HEALTH
1.7 PESTICIDE RESIDUE
1.8 MAXIMUM RESIDUE LEVEL (MRLS) OF PESTICIDE
1.9 PESTICIDE RESIDUE ANALYSIS-AN OVERVIEW
1.10 SAMPLE PREPARATION TECHNIQUES
1.10.1 Quick, Easy, Che ap, Effec ti ve, Rugged, and Safe (Qu ECh ERS) extrac tion method
1.11 CHROMATOGRAPHIC SEPARATION TECHNIQUES
1.11.1 Gas chromatography (GC)
1.11.2 Li qui d chr omatogr aphy (LC)
1.12 DETERMINATION TECHNIQUES
1.12.1 Li qui d chr omatogr aphy couple d with tande m mass spectrometr y (LC -MS/ MS)
1.13 MATRIX PROBLEMS IN PESTICIDE RESIDUE ANALYSIS
1.14 CALIBRATION TECHNIQUES
1.15 TARGET PESTICIDES AND PROBLEM ASSOCIATED WITH THIS STUDY
1.16 AIMS AND OBJECTIVES OF THE STUDY
CHAPTER 2 DEVELOPMENT OF Qu ECh ERS BASED EXTRACTION METHOD FOR UPLC-MS/MS DETERMINATION OF QUINOID NICLOSAMIDE (LDS) RESIDUE IN WATER, SOIL AND RIC E SAMPLES
2.1 INTRODUCTION
2.2 MATERIALS AND METHODS
2.2.1 Che micals and re agents
2.2.2 Appar atus for sample pre paration
2.2.3 Chromatogr aphic and mass spectrometr y c ondi tion
2.2.4 Sample pre paration
2.2.5 Method vali dation
2.3 RESULTS AND DISCUSSION
2.3.1 Opti mization of instrumental c ondi tions
2.3.2 Opti mization of LC mobile phase solve nts
2.3.3 Opti mization of c hromatographic c ondi tion
2.3.4 Opti mization of the e xtracti on and cle anup pr oce dure
2.4 VALIDATION OF THE METHOD
2.4.1 The Li nearity
2.4.2 Accurac y and precision
2.4.3 Li mits of de tection (LOD) and quanti ficati on (LOQ)
2.4.4 Matrix e ffect
2.4.5 Application to re al samples
Chapter 3 CONCLUSION
References
Acknowledgement
Resume
【參考文獻(xiàn)】:
期刊論文
[1]QuEChERS/液相色譜串聯(lián)質(zhì)譜法測(cè)定水產(chǎn)品中氯硝柳胺[J]. 劉伶俐,萬(wàn)譯文,伍遠(yuǎn)安,索紋紋,肖維. 食品工業(yè)科技. 2016(23)
[2]高效液相色譜-質(zhì)譜/質(zhì)譜聯(lián)用法檢測(cè)漁業(yè)水體中氯硝柳胺[J]. 萬(wàn)譯文,黃向榮,李小玲,陳湘藝,黃華偉. 分析試驗(yàn)室. 2015(01)
[3]氯代水楊胺對(duì)山丘釘螺實(shí)驗(yàn)室和現(xiàn)場(chǎng)殺螺效果研究[J]. 張劍鋒,朱明東,嚴(yán)曉嵐,蔣能明,林麗君,黃禮蘭,俞麗玲,葉曉東,聞禮永. 中國(guó)媒介生物學(xué)及控制雜志. 2014(01)
[4]雙水相浮選-HPLC法測(cè)定水中氯硝柳胺[J]. 傅海珍,謝菊,陳晶晶,楊曉雙,侯健,戚雪勇. 環(huán)境科學(xué)與技術(shù). 2013(09)
[5]10%氯代水楊胺可濕性粉劑現(xiàn)場(chǎng)滅螺效果觀察[J]. 張瑕,張華明,劉雄,榮先斌,楊蕊. 中國(guó)血吸蟲(chóng)病防治雜志. 2013(02)
[6]殺螺胺乙醇胺鹽在水稻和稻田中的殘留及消解動(dòng)態(tài)[J]. 伍一紅,龔道新,張素芳,周圣超. 農(nóng)業(yè)環(huán)境科學(xué)學(xué)報(bào). 2012(02)
[7]超聲萃取-高效液相色譜測(cè)定土壤中的氯硝柳胺[J]. 周穎,周藝彪,何明禎,王海銀,屈衛(wèi)東,姜慶五. 中國(guó)血吸蟲(chóng)病防治雜志. 2009(01)
[8]新型滅螺劑氯代水楊胺滅螺效果研究[J]. 徐興建,元藝,李桂玲,魏鳳華,趙云斌,涂祖武,劉敏,曹慕民,何匯,范宏萍. 中國(guó)血吸蟲(chóng)病防治雜志. 2007(05)
[9]不同樣品的氯硝柳胺乙醇膠鹽可濕性粉劑的殺螺效果與質(zhì)量比較[J]. 戴建榮,陳昌,梁幼生,張燕萍,鄭育賢,房文. 中國(guó)血吸蟲(chóng)病防治雜志. 1998(02)
[10]氯硝柳胺對(duì)魚(yú)類和溞類的毒性研究[J]. 修瑞琴,陳昌,許永香,高世榮,任改英,鄭靜. 中國(guó)血吸蟲(chóng)病防治雜志. 1996(06)
本文編號(hào):3477806
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