CN109580928A - 原料奶三种快速前处理方法 - Google Patents
原料奶三种快速前处理方法 Download PDFInfo
- Publication number
- CN109580928A CN109580928A CN201710895098.5A CN201710895098A CN109580928A CN 109580928 A CN109580928 A CN 109580928A CN 201710895098 A CN201710895098 A CN 201710895098A CN 109580928 A CN109580928 A CN 109580928A
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- China
- Prior art keywords
- precipitation method
- chloroform
- trichloroacetic acid
- lead
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000008267 milk Substances 0.000 title claims abstract description 46
- 235000013336 milk Nutrition 0.000 title claims abstract description 46
- 210000004080 milk Anatomy 0.000 title claims abstract description 46
- 238000002203 pretreatment Methods 0.000 title claims description 5
- 239000002994 raw material Substances 0.000 title abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 50
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000001556 precipitation Methods 0.000 claims abstract description 27
- 238000001514 detection method Methods 0.000 claims abstract description 22
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 claims abstract description 19
- -1 acetate lead Chemical compound 0.000 claims abstract description 16
- 238000003916 acid precipitation Methods 0.000 claims abstract description 14
- 238000007689 inspection Methods 0.000 claims abstract description 9
- PNZVFASWDSMJER-UHFFFAOYSA-N acetic acid;lead Chemical compound [Pb].CC(O)=O PNZVFASWDSMJER-UHFFFAOYSA-N 0.000 claims abstract description 5
- 235000013305 food Nutrition 0.000 claims abstract description 5
- 238000003759 clinical diagnosis Methods 0.000 claims abstract description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 claims description 2
- 231100000614 poison Toxicity 0.000 claims description 2
- 239000002574 poison Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- GKQAMYKQNHQPDJ-UHFFFAOYSA-K potassium disodium hydrogen phosphate 2-hydroxy-2-oxoacetate Chemical compound P(=O)([O-])([O-])[O-].[Na+].[Na+].C(C(=O)O)(=O)O.[K+] GKQAMYKQNHQPDJ-UHFFFAOYSA-K 0.000 claims 2
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- XCJINYQGOKCIBK-UHFFFAOYSA-L potassium sodium dihydrogen phosphate 2-hydroxy-2-oxoacetate Chemical compound P(=O)(O)(O)[O-].[Na+].C(C(=O)O)(=O)[O-].[K+] XCJINYQGOKCIBK-UHFFFAOYSA-L 0.000 abstract 1
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- ZBHXIWJRIFEVQY-IHMPYVIRSA-N ceftiofur Chemical compound S([C@@H]1[C@@H](C(N1C=1C(O)=O)=O)NC(=O)\C(=N/OC)C=2N=C(N)SC=2)CC=1CSC(=O)C1=CC=CO1 ZBHXIWJRIFEVQY-IHMPYVIRSA-N 0.000 description 5
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- IEDVJHCEMCRBQM-UHFFFAOYSA-N trimethoprim Chemical compound COC1=C(OC)C(OC)=CC(CC=2C(=NC(N)=NC=2)N)=C1 IEDVJHCEMCRBQM-UHFFFAOYSA-N 0.000 description 5
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- DNXHEGUUPJUMQT-UHFFFAOYSA-N (+)-estrone Natural products OC1=CC=C2C3CCC(C)(C(CC4)=O)C4C3CCC2=C1 DNXHEGUUPJUMQT-UHFFFAOYSA-N 0.000 description 1
- XWTYSIMOBUGWOL-UHFFFAOYSA-N (+-)-Terbutaline Chemical compound CC(C)(C)NCC(O)C1=CC(O)=CC(O)=C1 XWTYSIMOBUGWOL-UHFFFAOYSA-N 0.000 description 1
- PROQIPRRNZUXQM-UHFFFAOYSA-N (16alpha,17betaOH)-Estra-1,3,5(10)-triene-3,16,17-triol Natural products OC1=CC=C2C3CCC(C)(C(C(O)C4)O)C4C3CCC2=C1 PROQIPRRNZUXQM-UHFFFAOYSA-N 0.000 description 1
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- AZSNMRSAGSSBNP-UHFFFAOYSA-N 22,23-dihydroavermectin B1a Natural products C1CC(C)C(C(C)CC)OC21OC(CC=C(C)C(OC1OC(C)C(OC3OC(C)C(O)C(OC)C3)C(OC)C1)C(C)C=CC=C1C3(C(C(=O)O4)C=C(C)C(O)C3OC1)O)CC4C2 AZSNMRSAGSSBNP-UHFFFAOYSA-N 0.000 description 1
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
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- 108090000790 Enzymes Proteins 0.000 description 1
- 229930182566 Gentamicin Natural products 0.000 description 1
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- OJMMVQQUTAEWLP-UHFFFAOYSA-N Lincomycin Natural products CN1CC(CCC)CC1C(=O)NC(C(C)O)C1C(O)C(O)C(O)C(SC)O1 OJMMVQQUTAEWLP-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- GCKMFJBGXUYNAG-HLXURNFRSA-N Methyltestosterone Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@](C)(O)[C@@]1(C)CC2 GCKMFJBGXUYNAG-HLXURNFRSA-N 0.000 description 1
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- 239000004098 Tetracycline Substances 0.000 description 1
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- 206010047700 Vomiting Diseases 0.000 description 1
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- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- IYNDLOXRXUOGIU-LQDWTQKMSA-M benzylpenicillin potassium Chemical compound [K+].N([C@H]1[C@H]2SC([C@@H](N2C1=O)C([O-])=O)(C)C)C(=O)CC1=CC=CC=C1 IYNDLOXRXUOGIU-LQDWTQKMSA-M 0.000 description 1
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- PROQIPRRNZUXQM-ZXXIGWHRSA-N estriol Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@H]([C@H](O)C4)O)[C@@H]4[C@@H]3CCC2=C1 PROQIPRRNZUXQM-ZXXIGWHRSA-N 0.000 description 1
- 229960003399 estrone Drugs 0.000 description 1
- JKQQZJHNUVDHKP-SZMVRVGJSA-N flurogestone acetate Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@]2(F)[C@H]1[C@H]1CC[C@@](C(C)=O)(OC(=O)C)[C@]1(C)C[C@@H]2O JKQQZJHNUVDHKP-SZMVRVGJSA-N 0.000 description 1
- 239000003008 fumonisin Substances 0.000 description 1
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- 229960005287 lincomycin Drugs 0.000 description 1
- OJMMVQQUTAEWLP-KIDUDLJLSA-N lincomycin Chemical compound CN1C[C@H](CCC)C[C@H]1C(=O)N[C@H]([C@@H](C)O)[C@@H]1[C@H](O)[C@H](O)[C@@H](O)[C@@H](SC)O1 OJMMVQQUTAEWLP-KIDUDLJLSA-N 0.000 description 1
- PSGAAPLEWMOORI-PEINSRQWSA-N medroxyprogesterone acetate Chemical compound C([C@@]12C)CC(=O)C=C1[C@@H](C)C[C@@H]1[C@@H]2CC[C@]2(C)[C@@](OC(C)=O)(C(C)=O)CC[C@H]21 PSGAAPLEWMOORI-PEINSRQWSA-N 0.000 description 1
- 229960002985 medroxyprogesterone acetate Drugs 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 229940091868 melamine Drugs 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229960001566 methyltestosterone Drugs 0.000 description 1
- 229960000282 metronidazole Drugs 0.000 description 1
- VAOCPAMSLUNLGC-UHFFFAOYSA-N metronidazole Chemical compound CC1=NC=C([N+]([O-])=O)N1CCO VAOCPAMSLUNLGC-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229960004927 neomycin Drugs 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- AFDCXHSYKIVOOQ-UHFFFAOYSA-K potassium;disodium;phosphate Chemical compound [Na+].[Na+].[K+].[O-]P([O-])([O-])=O AFDCXHSYKIVOOQ-UHFFFAOYSA-K 0.000 description 1
- 239000000186 progesterone Substances 0.000 description 1
- 229960003387 progesterone Drugs 0.000 description 1
- YJQZYXCXBBCEAQ-UHFFFAOYSA-N ractopamine Chemical compound C=1C=C(O)C=CC=1C(O)CNC(C)CCC1=CC=C(O)C=C1 YJQZYXCXBBCEAQ-UHFFFAOYSA-N 0.000 description 1
- 229940074095 ractopamine Drugs 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229960000268 spectinomycin Drugs 0.000 description 1
- UNFWWIHTNXNPBV-WXKVUWSESA-N spectinomycin Chemical compound O([C@@H]1[C@@H](NC)[C@@H](O)[C@H]([C@@H]([C@H]1O1)O)NC)[C@]2(O)[C@H]1O[C@H](C)CC2=O UNFWWIHTNXNPBV-WXKVUWSESA-N 0.000 description 1
- 229960000195 terbutaline Drugs 0.000 description 1
- 229960003604 testosterone Drugs 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- OTVAEFIXJLOWRX-NXEZZACHSA-N thiamphenicol Chemical compound CS(=O)(=O)C1=CC=C([C@@H](O)[C@@H](CO)NC(=O)C(Cl)Cl)C=C1 OTVAEFIXJLOWRX-NXEZZACHSA-N 0.000 description 1
- 229960003053 thiamphenicol Drugs 0.000 description 1
- JTSDBFGMPLKDCD-XVFHVFLVSA-N tilmicosin Chemical compound O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CCN1C[C@H](C)C[C@H](C)C1)CO[C@H]1[C@@H]([C@H](OC)[C@H](O)[C@@H](C)O1)OC)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O JTSDBFGMPLKDCD-XVFHVFLVSA-N 0.000 description 1
- 229960000223 tilmicosin Drugs 0.000 description 1
- MEHHPFQKXOUFFV-OWSLCNJRSA-N trenbolone Chemical compound C1CC(=O)C=C2CC[C@@H]([C@H]3[C@@](C)([C@H](CC3)O)C=C3)C3=C21 MEHHPFQKXOUFFV-OWSLCNJRSA-N 0.000 description 1
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- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
- G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biomedical Technology (AREA)
- Hematology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Urology & Nephrology (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Cell Biology (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
本发明公开了三种原料奶前处理方法。三种前处理方法包括：乙酸铅沉淀法、三氯乙酸沉淀法和氯仿沉淀法。所述乙酸铅沉淀法是指在原料奶中加入乙酸铅溶液，混匀后再加入草酸钾‑磷酸二氢钠溶液，再次混匀后，离心获取上清液，作为待测样。所述三氯乙酸沉淀法是指在原料奶中加入三氯乙酸固体，混匀后离心获取上清液。上清液中加入氢氧化钠溶液，混匀后再次离心，所得上清液作为待测样。所述氯仿沉淀法是指在原料奶中加入氯仿，混匀后离心，取上清液待测样。本发明有效减少了奶样中干扰物质对检测结果的影响，简化了混匀、离心操作步骤，可显著提高检测的效率和准确度。可用于临床诊断、检验检疫、食品安全检测、司法鉴定、药品检测、毒品检测等多个领域。
Description
技术领域
本发明涉及原料奶三种快速前处理方法，具体涉及三种依据待测目标物不同理化性质研发的奶样前处理方法，属于生物医学技术领域。
背景技术
乳及乳制品营养丰富，但在动物饲养过程中存在抗生素、激素滥用以及毒素的污染，导致乳类食品中抗生素、激素、毒素等化学指标污染。对原料奶中化学污染物进行检测，可有效控制原料奶的质量，提高后续乳制品的安全性。
基于酶联免疫检测原理的测定方法由于其灵敏度高、特异性强，成本低廉的特点在乳品化学污染指标检测领域得到迅速发展，其中胶体金免疫层析检测技术是当前市场化应用最为成熟的产品之一。对于乳品中化学污染指标的胶体金检测试纸大多采用直接上样的方式，由于奶样成份复杂，明显制约了试纸检测灵敏度及准确性。同时，实验室奶样前处理步骤繁琐且涉及专业设备，不利于在现场环境展开操作。
发明内容
本发明针对上述胶体金快速检测乳品中化学污染物的不足，公开了原料奶三种快速前处理方法，目的是提高原料奶前处理效率，去除原料奶中的干扰物质，增进现有胶体金免疫检测产品测定乳品中化学污染指标的灵敏度与准确性。为了达到上述目的，本发明采用如下技术方案：
所述三种前处理方法包括：乙酸铅沉淀法、三氯乙酸沉淀法和氯仿沉淀法。
所述乙酸铅沉淀法是指在原料奶中加入乙酸铅溶液，混匀后加入草酸钾-磷酸氢二钠溶液，再次混匀后，离心获取上清液，作为胶体金检测卡待测样。
所述三氯乙酸沉淀法是指在原料奶中加入三氯乙酸固体，混匀后离心获取上清液。上清液中加入氢氧化钠溶液，混匀后再次离心，所得上清液作为胶体金检测卡待测样。
所述氯仿沉淀法是指在原料奶中加入氯仿，混匀后离心，取上清液作为胶体金检测卡待测样。
本发明所提供的原料奶三种快速前处理方式可用于临床诊断、检验检疫、食品安全检测、司法鉴定、毒品检测等诸多领域，具有广阔的市场前景。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，根据这些附图获得的其它附图都属于本发明保护的范围。
图1为本发明所述乙酸铅沉淀法处理奶样后与直接上样免疫层析结果对比
附图中，各标号所代表的材料列表如下：
1、乙酸铅沉淀法预处理奶样后免疫层析结果；2、直接上样免疫层析检测结果
图2为本发明所述三氯乙酸沉淀法处理奶样后与直接上样免疫层析结果对比
附图中，各标号所代表的材料列表如下：
1、三氯乙酸沉淀法预处理奶样后免疫层析结果；2、直接上样免疫层析检测结果
图3为本发明所述氯仿沉淀法处理奶样后与直接上样免疫层析结果对比
附图中，各标号所代表的材料列表如下：
1、氯仿沉淀法预处理奶样后免疫层析结果；2、直接上样免疫层析检测结果
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1，本发明所述乙酸铅沉淀法处理氯霉素加标奶样
所需试剂：1、20％乙酸铅溶液，配制方法：20g乙酸铅溶于水，并定容至100ml；2、草酸钾-磷酸氢二钠溶液，配制方法：草酸钾3g、磷酸氢二钠7g溶解于水并定容至100ml。
操作步骤：①分别配制1ml氯霉素加标浓度依次为0.6、0.3、0.15ppb及空白对照的原料奶；②每管加入100μl乙酸铅溶液，涡旋振荡1min；③；每管加入20μl草酸钾-磷酸氢二钠溶液，涡旋振荡1min；④3000rpm，离心3min；⑤吸取上清液用于氯霉素胶体金检测卡检测；⑥判断检测结果。
实验结果：经乙酸铅沉淀法处理的奶样相同加标浓度下信号响应比直接上样检测结果更灵敏。如图1，a、b、c、d组依次为氯霉素加标0.6、0.3、0.15ppb及空白对照经乙酸铅沉淀法预处理奶样后胶体金法测定结果；a1、b1、c1、d1组依次为氯霉素加标0.6、0.3、0.15ppb及空白对照直接上样胶体金法测定结果；图中可见相同加标浓度下，乙酸铅沉淀法预处理后测定T线比C线减弱更明显，提示信号响应更为灵敏。
所述判断检测结果，规则如下：
阳性：当质控区(C)显示出条带，而检测区(T)不显色或显色明显弱于C线，判为阳性，用“+”表示，如图1a、1b、1c、1a1、1b1。
阴性：当质控区(C)和检测区(T)均显示出条带且强度一致，判为阴性，用“-”表示，如图1d、1c1、1d1。
所述乙酸铅沉淀法适用于乳品中对重金属稳定的化学污染指标检测项目，如：氯霉素、磺胺二甲基嘧啶、林可霉素、红霉素、甲硝唑、伊维菌素、甲砜霉素、地塞米松、卡那霉素、替米考星、伏马菌素、雌二醇、睾酮、己烯雌酚、雌酮、甲基睾酮、醋酸氟孕酮等。
实施例2，本发明所述三氯乙酸沉淀法处理甲氧苄啶加标奶样
所需试剂：1、三氯乙酸；2、氢氧化钠溶液；配制方法：称取20g氢氧化钠溶解于水并定容至100ml。
操作步骤：①分别配制1ml甲氧苄啶加标浓度依次为200、100、50ppb及空白对照的原料奶②每管分别加入20mg三乙酸，涡旋振荡1min；③3000rpm离心3min；④吸取300μl上清液与2.5μl氢氧化钠溶液混合，涡旋30s；⑤吸取上清液用于免疫层析检测；⑥判断检测结果。
实验结果：经三氯乙酸沉淀法处理的奶样相同加标浓度下信号响应比直接上样检测结果更灵敏。如图2，a、b、c、d组依次为空白对照、甲氧苄啶加标50、100、200ppb经三氯乙酸沉淀法预处理奶样后胶体金法测定结果；a1、b1、c1、d1组依次为空白对照以及甲氧苄啶加标50、100、200ppb胶体金法测定结果；图中可见相同加标浓度下，三氯乙酸沉淀法预处理奶样后测定结果信号强度更强，T线随加标浓度梯度变化更为显著，提示信号响应更为灵敏。
所述判断检测结果，规则如下：
阳性：当质控区(C)显示出条带，而检测区(T)不显色或显色明显弱于C线，判为阳性，用“+”表示，如图2b、2c、2d、2b1、2c1、2d1。
阴性：当质控区(C)和检测区(T)均显示出条带且强度一致，或者质控区(C)弱于检测区(T)，判为阴性，用“-”表示，如图2a、2a1。
所述三氯乙酸沉淀法适用于乳品中对酸碱稳定的抗生素检测项目，如：泰勒菌素、庆大霉素、达佛沙星、甲氧苄啶、三聚氰胺、玉米赤霉醇、孕酮、莱克多巴胺、醋酸甲羟孕酮等。
实施例3，本发明所述氯仿沉淀法处理头孢噻呋加标奶样
所需试剂：氯仿；
操作步骤：①分别配制1ml加标浓度依次为10、2、2.2ppb及空白对照的头孢噻呋加标奶样；②分别加入1ml氯仿，涡旋振荡3min；③8000rpm下离心3min；④吸取上清液用于免疫层析检测；⑤判断检测结果。
实验结果：经氯仿沉淀法处理的奶样相同加标浓度下信号响应比直接上样检测结果更灵敏。如图3，a、b、c、d组依次为加标10、5、2.5ppb的头孢噻呋及空白对照经氯仿沉淀法预处理奶样后胶体金法测定结果；a1、b1、c1、d1组依次为加标10、5、2.5ppb的头孢噻呋及空白对照直接上样胶体金法测定结果；图中可见相同加标浓度下，氯仿沉淀法T线比C线减弱更明显，提示信号响应更为灵敏。
所述判断检测结果，规则如下：
阳性：当质控区(C)显示出条带，而检测区(T)不显色或显色明显弱于C线，判为阳性，用“+”表示，如图3a、3b、3c、3a1、3b1、3c1。
阴性：当质控区(C)和检测区(T)均显示出条带且强度一致，判为阴性，用“-”表示，如图3d、3d1。
所述氯仿沉淀法适用于乳品中对氯仿稳定的抗生素检测项目，如：头孢噻呋、四环素、青霉素G钾、大观霉素、(双氢)链霉素、新霉素、四环素、盐酸克伦特罗、特布他林、呕吐毒素、磺胺二甲基嘧啶、T-2毒素、雌三醇、群勃龙等。
以上对本发明实施例所提供的三种原料奶样前处理方法进行了详细介绍，可有效减少奶样中干扰物质对检测结果影响，提高检出率，适用于现场配套使用。本发明所提供的三种奶样前处理方式，可用于临床诊断、检验检疫、食品安全检测、司法鉴定、药品、毒品检测等领域。
本文中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处，综上所述，本说明书内容不应理解为对本发明的限制。
Claims (5)
1.三种奶样前处理方法，乙酸铅沉淀法、三氯乙酸沉淀法和氯仿沉淀法。
2.根据权利要求1所述的乙酸铅沉淀法，其特征在于涉及试剂包括：1、20％乙酸铅溶液；2、草酸钾-磷酸氢二钠溶液。所述20％乙酸铅溶液由20g乙酸铅溶于水，并定容至100ml配制而成；所述草酸钾-磷酸氢二钠溶液由草酸钾3g、磷酸氢二钠7g溶解于水并定容至100ml配制而成。
3.根据权利要求1所述的三氯乙酸沉淀法，其特征在于涉及试剂包括：1、三氯乙酸；2、氢氧化钠溶液。所述三氯乙酸为固体颗粒，现用现称。所述氢氧化钠溶液由20g氢氧化钠溶解于水并定容至100ml配制而成。
4.根据权利要求1所述的氯仿沉淀法，其特征在于涉及试剂为氯仿。
5.一种前处理权利要求1-4任一项所述的前处理方法，其包括步骤；
1)乙酸铅沉淀法涉及乙酸铅与草酸钾-磷酸氢二钠投加量及次序；
2)三氯乙酸沉淀法涉及三氯乙酸与氢氧化钠投加量及次序；
3)氯仿沉淀法涉及氯仿的投加量；
本发明所述三种前处理方法可用于临床诊断、检验检疫、食品安全检测、司法鉴定、毒品检测等诸多领域。
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