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1.
建立了超高效液相色谱-串联质谱法测定水产品中卡巴氧(CBX),喹烯酮(QCT)、乙酰甲喹(MEQ)、哇噁啉-2-羟酸(QCA),3-甲基喹噁啉-2-羧酸(MQCA) 5种化合物残留的分析方法.样品分别采用乙酸乙酯-乙腈(50:50)混合溶液、磷酸盐缓冲液分步提取,正己烷净化,以甲醇-乙腈(11:3)混合溶液和0.1%甲...  相似文献   

2.
建立了牛奶和奶粉中卡巴氧代谢物喹喔啉-2-羧酸(QCA)和喹乙醇代谢物3-甲基喹喔啉-2-羧酸(MQCA)残留量的液相色谱-串联质谱测定方法。将样品经0.6%(体积分数)的甲酸溶液进行消化,用Tris缓冲溶液调节pH后,加入Protease蛋白酶进行酶解,样品溶液用0.3 mol/L HCl溶液酸化后,采用阴离子交换固相萃取柱Oasis MAX进行净化和富集。分析样品以0.1%(体积分数)的甲酸溶液-甲醇-乙腈为流动相,经Inertsil ODS-3色谱柱分离,采用负离子扫描,在LC-MS/MS多反应监测模式下进行定性及定量分析。喹口恶啉-2-羧酸和3-甲基喹口恶啉-2-羧酸的方法测定下限牛奶为0.5μg/kg,奶粉为4.0μg/kg。对牛奶在0.5~5.0μg/kg,奶粉在4.0~40.0μg/kg添加水平的平均回收率为68.2%~82.5%,RSD为3.4%~12%。  相似文献   

3.
本文建立了猪、鸡、鱼肌肉及猪、鸡肝脏组织中喹乙醇代谢残留标识物3-甲基喹喔啉-2-羧酸残留量的高效液相色谱分析方法.样品在酸性环境水解,经乙酸乙酯、磷酸盐缓冲溶液依次提取,Oasis MAX固相萃取柱净化,高效液相色谱紫外测定(HPLC-UV).3-甲基喹喔啉-2-羧酸标准曲线相关系数(r2)为0.9992(10~1 000 μg/L);不同动物组织样品中3-甲基喹喔啉-2-羧酸工作曲线相关系数(r)为0.9995~0.9997(2~100 μg/kg).在2~100 μg/kg浓度范围,3-甲基喹喔啉-2-羧酸回收率为69%~104%,日内相对标准偏差<15%,日间相对标准偏差<20%.检出限(CCα)为1.2~4.3 μg/kg,定量限(CCβ)为2.0~5.6 μg/kg.  相似文献   

4.
建立了动物源食品猪肉、鸡肉和鱼肉中喹喔啉类兽药喹乙醇(OLQ)、卡巴氧(CBX)的高效液相色谱-串联质谱测定方法。样品经0.1 mol/L磷酸二氢钠 (pH 6.0)溶液提取,Oasis HLB 固相萃取柱净化,流动相定容后,采用Waters Xterra MS C18柱(5 μm,150 mm×2.1 mm) 分离,以乙腈-0.2%甲酸为流动相进行梯度洗脱,以串联质谱在多反应监测(MRM)正离子模式下检测,基质外标法定量。结果表明,喹乙醇和卡巴氧在质量浓度为1~20 ng/mL范围内线性关系良好,相关系数为0.998 1~0.999 9;各基质在0.2、0.4、2.0 μg/kg 3个加标水平下,喹乙醇和卡巴氧的回收率为70%~93%,相对标准偏差为1.9%~16.7%,定量下限(S/N≥10)均为0.2 μg/kg。应用建立的方法对猪肉、鸡肉、鱼肉样品各20个进行检测,并与国标方法进行比较,结果满意。该方法简单、灵敏、稳定,可满足猪肉、鸡肉和鱼肉中喹乙醇、卡巴氧残留的检测与确证需要。  相似文献   

5.
建立了动物源食品猪肉、鸡肉和鱼肉中喹喔啉类兽药喹乙醇(OLQ)、卡巴氧(CBX)的高效液相色谱-串联质谱测定方法。样品经0.1 mol/L磷酸二氢钠(pH 6.0)溶液提取,Oasis HLB固相萃取柱净化,流动相定容后,采用Waters Xterra MS C18柱(5μm,150 mm×2.1 mm)分离,以乙腈-0.2%甲酸为流动相进行梯度洗脱,以串联质谱在多反应监测(MRM)正离子模式下检测,基质外标法定量。结果表明,喹乙醇和卡巴氧在质量浓度为1~20 ng/mL范围内线性关系良好,相关系数为0.998 1~0.999 9;各基质在0.2、0.4、2.0μg/kg 3个加标水平下,喹乙醇和卡巴氧的回收率为70%~93%,相对标准偏差为1.9%~16.7%,定量下限(S/N≥10)均为0.2μg/kg。应用建立的方法对猪肉、鸡肉、鱼肉样品各20个进行检测,并与国标方法进行比较,结果满意。该方法简单、灵敏、稳定,可满足猪肉、鸡肉和鱼肉中喹乙醇、卡巴氧残留的检测与确证需要。  相似文献   

6.
郑玲  吴玉杰  李湧  李丽华 《色谱》2012,30(7):660-664
建立了动物源食品中喹喔啉类药物代谢残留标识物3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸的高效液相色谱-串联质谱检测方法。样品在酸性环境水解,经乙酸乙酯、磷酸盐缓冲液依次提取,Oasis MAX固相萃取小柱净化,用Waters Xterra MS C18柱(150 mm×2.1 mm, 5 μm)分离,以甲醇-0.2%甲酸为流动相梯度洗脱,采用多反应监测(MRM)正离子模式检测,内标法定量。各物质在1.0~20.0 μg/L范围内线性关系良好,相关系数均不低于0.9996; 3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸在0.1、0.2、1.0 μg/kg加标水平的回收率为62.4%~118%,相对标准偏差为1.48%~28.1%;定量限(以信噪比≥10计)为0.1 μg/kg。该方法简单、灵敏、稳定,可满足猪肉、猪肝、鸡肉、鸡肝、鱼、虾等动物源食品中3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸残留的检测与确证需要。  相似文献   

7.
魏敏芝  万建春  张富生  潘华 《色谱》2019,37(10):1059-1063
建立了高效液相色谱-串联质谱同时定量和确证猪肉中3-甲基喹喔啉-2-羧酸(MQCA)残留量的检测方法。试样用0.3 mol/L盐酸溶液水解提取,加入乙腈和乙酸乙酯萃取,再用0.1 mol/L氢氧化钠溶液反萃取,阴离子交换固相萃取柱净化,经Agilent Eclipse Plus C18柱(50 mm×3.0 mm,1.8 μm)分离,采用液相色谱-串联质谱仪检测,基质匹配添加标准曲线定量。MQCA在1.0~50 μg/L范围内线性相关系数大于0.99,在0.5、1.0、5.0 μg/kg加标水平下其回收率为90.5%~119.6%,相对标准偏差为3.14%~4.22%。方法可用于猪肉中MQCA残留量的快速定量和确证检测。  相似文献   

8.
采用液相色谱-串联质谱(HPLC—MS/MS)法测定鸡组织(肌肉、肝、肾)中喹烯酮标示残留物3-甲基喹噁啉-2-羧酸的含量。组织匀浆样品经碱水解、液液萃取,采用HPLC—MS/MS电喷雾电离(ESI),正离子模式,多反应监测(MRM),以喹噁啉-2-羧酸为内标进行定量。检出限为5μg/kg。  相似文献   

9.
建立了高效液相色谱-质谱(LC-MS/MS)检测水产品中喹乙醇代谢物3甲-基-喹恶啉-2羧-酸(MQCA)的残留分析方法。样品先用Protease蛋白酶酶解,然后用乙酸乙酯萃取目标物,氮气吹干后用流动相溶解残渣,以甲醇、乙腈和0.1%甲酸溶液作为流动相,液相色谱串联电喷雾质谱在正离子模式下测定。MQCA在1~100μg/kg范围内线性关系良好(r0.999)。在2、4、8μg/kg3个添加水平上,回收率在82.5%~87.5%,相对标准偏差为4.5%~5.1%(n=6),定量限为1μg/kg。方法已用于水产品中喹乙醇代谢物的残留分析。  相似文献   

10.
以草鱼、南美白对虾、中华绒鳌蟹为样品,建立了喹烯酮(QCT)和喹赛多(CYA)及其主要代谢物脱二氧喹烯酮(BDQCT)、3-甲基喹啉-2-羧酸(MQCA)、脱二氧喹赛多(BDCYA)和喹啉-2-羧酸(QCA)多残留的高效液相色谱-串联质谱(HPLC-MS/MS)确证检测方法。组织样品经乙腈-乙酸乙酯(1∶1)、盐酸溶液分步提取,Oasis MAX固相萃取柱净化,以甲醇、乙腈和0.1%甲酸溶液为流动相,经Waters XBridge C18色谱柱分离后,采用HPLC-MS/MS仪进行测定。采取正离子选择反应监测模式检测,外标法定量。结果表明,喹烯酮和喹赛多及其主要代谢物的响应值与其质量浓度在2~500μg/L范围内线性关系良好。在加标浓度为5~50μg/kg范围内,6种待测物的平均回收率为76.3%~94.2%,相对标准偏差为4.2%~11.7%。方法的检出限为0.5~1.6μg/kg,定量下限为2.0~5.0μg/kg。该方法适用于水产品中QCT和CYA及其主要代谢物残留的确证检测和同时定量分析。  相似文献   

11.
The reactions of N-substituted hydroxylamines with alkenals serve as a method for the synthesis of the corresponding 2-substituted 3(5)-hydroxyisoxazolidines. The reaction pathway is determined by the nature of the substituent attached to the nitrogen atom. Ring-chain isomerism has been detected in these newly obtained compoundsTranslated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1270–1276, September, 1987.  相似文献   

12.
The values of activation parameters in uncured and cured epoxy resins, rubbers, and blends thereof are investigated. The dependences of activation energy and adhesion strength of epoxy-rubber compositions on rubber content are determined. The correlation of adhesion and activation energy values for polyurethane rubber and epoxy-rubber compositions is shown.  相似文献   

13.
Aroyl- and acetylhydrazones of acet- (I) and benzaldehydes (IV) and benzoylhydrazones of acet- (II) and benzaldehydes (III) were studied by x-ray structural and quantum-chemical methods in order to establish their structures. Compund (I) was the EEZ structure in the crystal. Calculations and spectral data showed that the EEE form occurs in nonpolar solvents and in the gas phase. According to crystallographic data molecules (I)–(IV) are the E-isomers (relative to the N-N bond) and the hydrazone fragments are planar. Intermolecular N-H...O H-bonds from in the crystals. The data obtained suggest that the majority of acylhydrazones are conformationally rigid on dissolution although exceptions do occur. Apparently the reasons for the difference of acetyl- and benzoylhydrazones in electrocarboxylation reactions are electronic and not steric factors.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 1, pp. 75–81, January, 1991.  相似文献   

14.
Conclusions The mass and NMR spectra of haplophyllidine, perforine, and their derivatives have been studied. The influence of the open and cyclic forms of the molecular ion on the nature of the fragmentation has been discussed. The main routes of fragmentation of the compounds considered are due to the presence of substituents at C8 and C4.Khimiya Prirodnykh Soedinenii, Vol. 5, No. 4, pp. 273–279, 1969  相似文献   

15.
Triazenide [M(eta2-1,3-ArNNNAr)P4]BPh4 [M = Ru, Os; Ar = Ph, p-tolyl; P = P(OMe)3, P(OEt)3, PPh(OEt)2] complexes were prepared by allowing triflate [M(kappa2-OTf)P4]OTf species to react first with 1,3-ArN=NN(H)Ar triazene and then with an excess of triethylamine. Alternatively, ruthenium triazenide [Ru(eta2-1,3-ArNNNAr)P4]BPh4 derivatives were obtained by reacting hydride [RuH(eta2-H2)P4]+ and RuH(kappa1-OTf)P4 compounds with 1,3-diaryltriazene. The complexes were characterized by spectroscopy and X-ray crystallography of the [Ru(eta2-1,3-PhNNNPh){P(OEt)3}4]BPh4 derivative. Hydride triazene [OsH(eta1-1,3-ArN=NN(H)Ar)P4]BPh4 [P = P(OEt)3, PPh(OEt)2; Ar = Ph, p-tolyl] and [RuH{eta1-1,3-p-tolyl-N=NN(H)-p-tolyl}{PPh(OEt)2}4]BPh4 derivatives were prepared by allowing kappa1-triflate MH(kappa1-OTf)P4 to react with 1,3-diaryltriazene. The [Os(kappa1-OTf){eta1-1,3-PhN=NN(H)Ph}{P(OEt)3}4]BPh4 intermediate was also obtained. Variable-temperature NMR studies were carried out using 15N-labeled triazene complexes prepared from the 1,3-Ph15N=N15N(H)Ph ligand. Osmium dihydrogen [OsH(eta2-H2)P4]BPh4 complexes [P = P(OEt)3, PPh(OEt)2] react with 1,3-ArN=NN(H)Ar triazene to give the hydride-diazene [OsH(ArN=NH)P4]BPh4 derivatives. The X-ray crystal structure determination of the [OsH(PhN=NH){PPh(OEt)2}4]BPh4 complex is reported. A reaction path to explain the formation of the diazene complexes is also reported.  相似文献   

16.
17.
Reaction of the proligand Ph2PN(SiMe3)2 (L1) with WCl6 gives the oligomeric phosphazene complex [WCl4(NPPh2)]n, 1 and subsequent reaction with PMe2Ph or NBu4Cl gives [WCl4(NPPh2)(PMe2Ph)] (2) or [WCl5(NPPh2)][NBu4] (3), respectively. DF calculations on [WCl5(NPPh2)][NBu4] show a W=N double bond (1.756 A) and a P-N bond distance of 1.701 A, which combined with the geometry about the P atom suggests, there is no P-N multiple bonding. Reaction of L1 with [ReOX3(PPh3)2] in MeCN (X = Cl or Br) gives [ReX2(NC(CH3)P(O)Ph2)(MeCN)(PPh3)](X = Cl, 4, X = Br, 5) which contains the new phosphorylketimido ligand. It is bound to the rhenium centre with a virtually linear Re-N-C arrangement (Re-N-C angle = 176.6 degrees, when X = Cl) and there is multiple bonding between Re and N (Re-N = 1.809(7) A when X = Cl). The proligand Ph2PNHNMe2(L2H) reacts with [(C5H5)TiCl3] to give [(C5H5)TiCl2(Me2NNPPh2)] (6). An X-ray crystal structure of the complex shows the ligand (L2) is bound by both nitrogen atoms. Reaction of the proligands Ph2PNHNR2[R2 = Me2 (L2H), -(CH2CH2)2NCH3 (L3H), (CH2CH2)2CH2 (L4H)] with [{RuCl(mu-Cl)(eta6-p-MeC6H4iPr)}2] gave [RuCl2(eta6-p-MeC6H4iPr)L] {L = L2H (7), L3H (8), L4H (9)}. The X-ray crystal structures of 7-9 confirmed that the phosphinohydrazine ligand is neutral and bound via the phosphorus only. Reaction of complexes 7-9 with AgBF4 resulted in chloride ion abstraction and the formation of the cationic species [RuCl(6-p-MeC6H4iPr)(L)]+ BF4- {(L = L2H (10), L3H (11), L4H (12)}. Finally, reaction of complex 6 with [{RuCl(mu-Cl)(eta6-p-MeC6H4iPr)}2] gave the binuclear species [(eta6-p-MeC6H4iPr)Cl2Ru(mu2,eta3-Ph2PNNMe2)TiCl2(C5H5)], 13.  相似文献   

18.
Selenium dioxide and osmium tetroxide are effective reagents and catalysts for olefin oxidation, although, owing to their toxicity, reservations remain as to their applicability.[1] We are therefore seeking more easily handled metal oxides that are soluble in organic solvents and that are as effective as osmium tetroxide in carrying out stereospecific cis hydroxylation of olefins. The rhenium(VII ) oxide 1 , which has meanwhile become readily accessible, is a favorable candidate.[2]  相似文献   

19.
20.
朱劲波  马立群  梁飞  苗迎春  王立民 《应用化学》2015,32(11):1221-1230
Ti-V基储氢合金在室温、常压下即可表现出良好的储氢特性,且质量储氢容量明显高于传统AB5型储氢合金,从而在氢气的精制和回收、运输和储存及热泵等方面有较早的应用。 此外,在混合气体分离、核反应堆中处理氢的同位素、镍氢电池及燃料电池负极材料等方面也得到了广泛的研究与关注。 基于目前Ti-V基储氢合金的研究现状,概述了该类合金的优势、限制性因素(包括成因)及改性手段。 此外,为了进一步理解Ti-V基合金储氢机理、构建合金组分与储氢特性之间的对应关系,本工作重点围绕Ti-V基储氢合金及其氢化物的结构、组分优化设计展开综述,并对其未来研究方向做出展望。  相似文献   

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