超高效液相色谱串联质谱法测定液态奶中氯霉素、甲砜霉素和氟苯尼考含量

建立超高效液相色谱串联质谱法测定液态奶中氯霉素、甲砜霉素和氟苯尼考的检测方法。样品经乙酸乙酯提取,Oasis MCX小柱净化,用色谱柱WATERS ACQUITY UPLC BEH C18(1.7um, 2.1mm*100mm)分离,同位素内标法定量。在优化条件下,该方法中氯霉素的最低检出限为0.05μg /kg,定量限为0.15μg /kg, 甲砜霉素和氟苯尼考的最低检出限为0.1μg /kg,定量限为0.3μg /kg, 平均回收率为80.4~105.4%,相对标准偏差为2.8~8.4%。该方法灵敏度高、回收率好,具有良好的净化效果,提升检测效率,适用于液态奶中氯霉素、甲砜霉素和氟苯尼考的同时检测。     

UPLC-MS/MS法测定乳制品中的氯霉素类药物

建立超高效液相色谱-串联质谱(UPLC-MS/MS)法测定乳与乳制品中氯霉素、甲砜霉素和氟苯尼考的检测方法。样品经乙腈及乙酸乙酯提取、正己烷脱脂、C18柱净化后,通过超高效液相色谱-质谱联用仪进行检测,内标法定量。各标准溶液在0.1～10μg/L范围内呈线性相关(r=0.999),不同基质样品中添加回收率为75%～114%,检出限为0.1μg/kg。结果表明,该方法是一种准确测定乳与乳制品中氯霉素、甲砜霉素和氟苯尼考的检测方法。     

气相色谱-串联质谱法同时测定肉制品中氯霉素、甲砜霉素残留

建立了肉制品中氯霉素、甲砜霉素的气相色谱串联质谱检测方法。样品经均质后,用乙酸乙酯提取,正己烷脱脂,弗罗里硅土小柱净化,衍生后用气相色谱串联质谱法检测,内标法定量。优化了二级质谱条件,包括离子对及碰撞电压。该方法检出限为氯霉素(CAP)0.02μg/kg,甲砜霉素(TAP)0.1μg/kg,加标回收率均在86%~97%之间,相对标准偏差(RSD)在3.8%~12.3%之间,在0.1~20 ng/mL范围内都呈现出良好线性关系。     

Captiva EMR-Lipid固相萃取结合高效液相色谱-串联质谱法同时测定猪肉中氯霉素类药物残留量

目的 建立Captiva EMR-Lipid固相萃取结合高效液相色谱-串联质谱法同时测定猪肉中氯霉素、甲砜霉素和氟苯尼考残留量的分析方法。方法 采用乙腈提取样品, 经Captiva EMR-Lipid固相萃取柱净化, 以甲醇-水为流动相, CNW Athena C18-WP色谱柱(100 mm×2.1 mm, 3 μm)进行分离, 采用电喷雾负离子扫描和多反应监测模式, 内标法定量。结果 氯霉素、甲砜霉素和氟苯尼考在0.5~20.0 ng/mL范围内呈现良好的线性关系(r＞0.9975), 方法的检出限为0.10~0.14 ?g/kg, 定量限为0.25~0.47 ?g/kg, 平均回收率为97.50%~117.00%, 相对标准偏差为5.55%~8.93%。结论 该方法简单快速、稳定可靠, 适用于猪肉中氯霉素、甲砜霉素和氟苯尼考的同时测定。     

液相色谱-质谱法测定乳及乳制品中氯霉素类抗生素的含量

目的建立液相色谱-质谱法测定乳及乳制品中氯霉素类抗生素的残留量。方法液态奶、酸奶、奶粉样本经乙酸乙酯提取,经Waters Sep-pak C_(18)固相萃取小柱净化,至Agilent C_(18)(150 mm×2.1 mm,5μm)色谱柱分离,以乙腈:水(50:50,V:V)为流动相进行等度洗脱。质谱法采用电喷雾离子源负离子模式和多反应监测模式测定,以内标法定量。结果氯霉素、甲砜霉素、氟苯尼考3种待测物质在0.1~20 ng/m L范围内线性关系良好,线性相关系数都在0.9995以上;氯霉素的检出限为0.011~0.021μg/kg,甲砜霉素的检出限为0.042~0.100μg/kg,氟苯尼考的检出限为0.010~0.018μg/kg;氯霉素在0.05、0.5和1μg/kg 3水平上的加标回收率为83.1%~95.6%,甲砜霉素在0.1、1和2μg/kg 3水平上的的加标回收率为80.2%~102.1%,氟苯尼考在0.05、0.5和1μg/kg 3水平上的的加标回收率为81.3%~103.5%;氯霉素的相对标准偏差为4.4%~6.4%,甲砜霉素的相对标准偏差为4.1%~7.1%,氟苯尼考的相对标准偏差为3.7%~6.6%。结论本方法准确灵敏,适用于乳及乳制品中氯霉素类抗生素残留量的测定。     

高效液相色谱-串联质谱法同时检测虾肉和猪肉中氯霉素、甲砜霉素、氟苯尼考和其代谢产物氟苯尼考胺残留

建立了高效液相色谱-串联质谱法同时检测虾肉和猪肉中氯霉素、甲砜霉素、氟苯尼考和其代谢产物氟苯尼考胺残留。以2%碱性乙酸乙酯提取,省去固相萃取(SPE)和液-液萃取(LPE)脱脂,浓缩后采用甲醇和5mmol/L乙酸铵以0.25 mL/min流速梯度洗脱,LC-MS/MS电喷雾电源(ESI),负离子,选择反应监测(SRM)模式检测。试验结果表明:4种药物在0.1~20μg/L的范围内线性良好,相关系数R2在0.9997~0.9998之间。在添加量为1.00~5.00μg/kg时,平均回收率在78.17%~99.86%之间,RSD在2.18%~9.27%之间。氯霉素、甲砜霉素、氟苯尼考和氟苯尼考胺的检出限分别为0.001,0.020,0.002,0.003μg/kg。     

液质联用法测定牛奶中氯霉素类药物残留

建立了牛奶中氯霉素、甲砜霉素和氟甲砜霉素多残留的高效液相色谱-串联四极杆质谱联用测定方法。样品经碱性乙腈超声提取,以MGⅢ-C18色谱柱(2.1×150 mm,5μm)分离,流动相为10 mmol/L乙酸铵水溶液和甲醇(梯度洗脱),流速0.25 m L/min。采用多反应监测负离子模式,可以同时对牛奶中的氯霉素、甲砜霉素和氟甲砜霉素进行定性和定量测定。方法的检出限为0.1μg/kg~0.3μg/kg。在0.3、3.0、10.0μg/kg 3个加标水平下,加标回收率为80.7%~93.6%,相对标准偏差为3.85%~9.35%。     

动物源性食品中氯霉素类药物残留量的测定

本文采用QuE-UPLC/MS/MS法测定猪肉、草鱼、牛奶、蜂蜜等动物源性食品中氯霉素、甲砜霉素的残留量。该方法使用乙腈作为提取溶剂,样品经搅匀、涡旋、振荡、离心、净化处理后上机分析。本方法的优点体现在样品前处理方法简易、省时,能够同时检测氯霉素和甲砜霉素两种目标组分,在节省了检测时间的同时降低了基质效应;氯霉素和甲砜霉素的回收率均可达到85%以上,确保了实验结果的准确性和重现性;氯霉素和甲砜霉素的检出限均为0.1μg/kg,优于《可食动物肌肉、肝脏和水产品中氯霉素、甲砜霉素和氟苯尼考残留量的测定液相色谱-串联质谱法》(GB/T 20756-2006)的检测方法。     

高效液相色谱-电喷雾电离串联质谱法测定鸡肉、鸡蛋中氯霉素、甲砜霉素和氟苯尼考药物残留量

目的建立高效液相色谱-电喷雾电离串联质谱法测定鸡肉和鸡蛋中氯霉素、甲砜霉素、氟苯尼考残留量的分析方法。方法准确称取5 g样品,添加同位素内标氯霉素-d5后,乙腈提取,LC-Si硅胶小柱净化,正己烷进一步除脂,0.22μm滤膜过滤后高效液相色谱-电喷雾电离串联质谱测定。采用负离子电喷雾电离源,多反应监测(multiple reaction monitoring,MRM)模式。结果氯霉素、甲砜霉素和氟苯尼考在0.5~200μg/L的系列浓度范围内线性良好,其线性方程分别为Y=0.880X-0.215,Y=0.032X-0.076和Y=0.108X-0.115,相关系数r~2均大于0.990;方法的检测限和定量限分别是0.05μg/kg和0.1μg/kg;在加标水平在0.1~5.0μg/kg的范围内,鸡肉基质中平均回收率在87.01%~117.8%之间,鸡蛋基质中平均回收率在80.74%~115.0%之间;方法的日内精密度相对标准偏差在4.02%~9.88%之间,日间精密度相对标准偏差在5.72%~12.78%之间。结论该方法简单易行,回收率好,灵敏度高,特异性好,能满足目前大多数日常检测和监督的需要。     

超高效液相色谱-串联质谱结合谱库检索快速测定鸡蛋中氯霉素、氟苯尼考和甲砜霉素残留

采用超高效液相色谱-三重四级杆/复合线性离子阱质谱(QTrap UPLC-MS/MS)技术结合谱库检索分析,建立了鸡蛋中氯霉素、氟苯尼考和甲砜霉素的快速检测确证方法。样品加入氯霉素-D5后,经乙腈提取,浓缩至干,3.00 mL水复溶,正己烷去脂净化,以乙腈-水为流动相,经Phenomenex Kinetex F5色谱柱(100 mm×3.0 mm,2.6 μm)分离,用QTrap UPLC-MS/MS进行多反应监测(MRM)、信息依赖性扫描(IDA)、增强子离子扫描(EPI)和谱库检索分析。氯霉素内标法定量,氟苯尼考、甲砜霉素外标法定量。结果表明,氯霉素和氟苯尼考在0.03~50.0 μg/L,甲砜霉素在0.06~50.0 μg/L的线性范围内线性关系良好,相关系数r>0.999;氯霉素、氟苯尼考和甲砜霉素在3个加标水平下,平均回收率为90.1%~120.0%,精密度为4.2%~11.9%,检出限为0.05~0.10 μg/kg。该方法高效、简便、准确,可用于鸡蛋中酰胺醇类抗生素定性和定量分析。     

Determination of Chloramphenicol in Honey, Shrimp, and Poultry Meat with Liquid Chromatography–Mass Spectrometry: Validation of the Method According to Commission Decision 2002/657/EC

Chloramphenicol (CAP) is an antibiotic used for the treatment of bacterial infections in human and veterinary medicine. The use of CAP was prohibited in the European Union in 1994. Control laboratories are required to use suitably validated analytical methods to check sample compliance with the regulation. A quantitative method based on liquid chromatography coupled to isotopic dilution tandem mass spectrometry was developed for the determination of chloramphenicol in honey, shrimp, and poultry meat. The experimental protocol consisted of a liquid–liquid extraction with ethyl acetate. Separation and detection were realized, respectively, by a 2690 Waters HPLC (Milford, MA, USA) and a Micromass Triple Quadrupole mass spectrometer (Micromass, Manchester, UK), equipped with an electrospray source. The effects of mobile-phase additives on the response of LC/ESI/MS were examined. Two different HPLC columns were tested: the X-Terra from Waters and the Alltima HP C18 HL from Alltech (Deerfield, IL, USA). A validation of the method was conducted according to the EU criteria for the analysis of chloramphenicol in foods. The decision limits (CCα) were 0.04, 0.03, 0.07 μg?kg^?1, and the detection capabilities (CCβ) were 0.05, 0.04, 0.08 μg?kg^?1 for honey, shrimp, and poultry meat, respectively. Those values are below the minimum required performance limit set at 0.3 μg?kg^?1 by the EU and 0.1 μg?kg^?1 by Belgium. Our protocol has the advantage to propose a unique extraction method working as well for honey, shrimp, and poultry meat, contrary to similar published methods in which a different extraction method is used for each type of matrix.     

Determination of Five Alkaloids of Pericarpium Papaveris in Hot Pot Broth Using Ultra-Performance Liquid Chromatography Coupled to Triple Quadruple Mass Spectrometry

Simultaneous determination of five alkaloids (morphine, codeine, noscapine, thebaine, and papaverine) of pericarpium papaveris in hot pot broth was established by ultra-performance liquid chromatography (UPLC) coupled to triple quadruple mass spectrometry (QqQ-MS). Water containing 0.1 mol/L hydrochloric acid was used as extraction solution and petroleum ether were used for fat removal. Then, the water-phase extracts were purified by an Oasis MCX cartridge. After separation by a BEH C18 (50?×?2.1 mm, 1.7 μm) column, five alkaloids were detected by mass spectrometry in the positive electrospray ionization with multiple reaction monitoring (MRM). The linear ranges were 0.1–10.0 μg/kg for morphine, codeine, and thebaine, as well as 0.01–1.0 μg/kg for papaverine and noscapine, respectively. The limits of quantification (LOQs) for morphine, codeine, and thebaine were 0.1 μg/kg and for papaverine and noscapine were 0.01 μg/kg. Mean recoveries at three spiked concentrations for the objectives were varied from 72.1 % to 124 %. The method was employed in real samples and demonstrated its rapidness and high sensibility.     

气相色谱-质谱联用测定白酒中的氨基甲酸甲酯和氨基甲酸乙酯

建立一种测定白酒中的氨基甲酸甲酯和氨基甲酸乙酯的气相色谱-质谱联用(gas chromatography-mass spectrometry,GC-MS)方法。GC-MS条件为：色谱柱HP-55%苯甲基硅氧烷(30.0m×0.25mm,0.25μm),进样1μL(分流比50:1),柱温170℃,质谱离子源温度230℃,四极杆温度150℃,全扫描方式的质量扫描范围m/z 30～500,溶剂延迟3min。样品采用氨基固相小柱萃取净化、氮吹浓缩定容。结果表明：氨基甲酸甲酯和氨基甲酸乙酯在2～30μg/mL范围内线性关系良好,相关系数为0.9923和0.9811,平均回收率为76.10%和75.43%,RSD为4.48%和4.00%。该方法可应用于白酒检测。     

Rapid detection of chloramphenicol in animal products without clean-up using LC-high resolution mass spectrometry

A rapid confirmatory and quantitative method using liquid chromatography-high resolution mass spectrometry (LC-HRMS) was developed to determine sub-μg/kg levels of chloramphenicol (CAP) in meat products. The sample plus deuterated chloramphenicol internal standard was homogenised, extracted with ethyl acetate, centrifuged and the supernatant evaporated to dryness. The residue was re-dissolved in methanol/5% ammonium acetate solution (20:80, v/v), defatted with hexane and directly injected into the LC-MS. Chromatographic separation was performed on a C(18) column using methanol/water (60:40, v/v) as the mobile phase. CAP was detected using selected ion monitoring of the high accurate mass of the molecular ion [M-H](-) of CAP using a LTQ-Orbitrap mass spectrometer in negative electrospray ionisation mode (ESI(-)). The limit of quantification of the method was 0.1?μg/kg using isotope internal standard. Recoveries of CAP spiked at levels of 0.1-1.0?μg/kg ranged from 73 to 99%, and the relative standard deviation ranged 3.9-8.1%.     

免疫亲和柱净化-HPLC法同时测定玉米制品中的赭曲霉毒素A和玉米赤霉烯酮

建立了同时测定玉米制品中赭曲霉毒素A和玉米赤霉烯酮的免疫亲和柱净化高效液相色谱方法。试样经乙腈-水溶液(体积比80?20)提取,复合免疫亲和柱富集和净化后,采用Syncronis C18色谱柱(250 mm×4.6 mm,5μm)固定相,以0.5%冰乙酸-乙腈-甲醇(体积比10?45?45)为流动相,等度洗脱,荧光检测器检测(Ex:333 nm,Em:470 nm)。结果表明:赭曲霉毒素A和玉米赤霉烯酮检出限分别为5.65×10-2μg/kg和4.53×10-1-μg/kg;标准曲线的线性范围分别为1~50 ng/mL(r=0.9999)和10~500 ng/mL(r=0.9999);3个不同水平的加标平均回收率为95.81%~98.31%,RSD值为1.24%~1.65%。20批试样中赭曲霉毒素A和玉米赤霉烯酮测定值分别为0.59~0.69μg/kg和3.84~5.22μg/kg,均无过量残留。该方法具有操作简便、灵敏度高、重现性佳等优点,适用于同时检测玉米制品中赭曲霉毒素A和玉米赤霉烯酮。     

高效液相色谱-串联质谱法测定动物源食品中氯霉素残留

目的建立高效液相色谱-串联质谱法测定几种动物源食品中氯霉素残留的方法。方法对《动物源食品中氯霉素残留量的测定高效液相色谱-串联质谱法》(农业部第781号公告)中的测定方法进行优化,样品经提取后经HLB固相萃取小柱净化,采用甲醇-水进行梯度洗脱,经Agilent Eclipse-plus C₁₈色谱柱(3.0 mm×100 mm,1.8μm)分离,采用多反应检测负离子模式进行定性及定量分析。结果在0.5~10.0 ng/mL范围内,氯霉素的浓度和色谱峰面积线性关系良好(r=0.9998),方法检出限为0.03μg/kg,定量限为0.1μg/kg,在1.0、2.0和5.0 ng/mL 3个水平的加标回收率为91.58%~109.52%,相对标准偏差小于7.5%。结论该方法快速、准确、灵敏,能满足几种动物源食品中氯霉素残留的测定。     

超高效液相色谱-串联质谱法测定鸡肉和猪肉中利尿剂残留量

目的:建立测定鸡肉和猪肉中违禁添加物呋塞米、螺内酯和布美他尼含量的超高效液相色谱-串联质谱法。方法:样品用乙酸乙酯提取后,经C₁₈粉净化。色谱柱为Hypersil GOLD C₁₈（1.9 μm,2.1 mm×50 mm）,流动相为乙腈和0.1%甲酸水,梯度洗脱,流速为0.4 mL/min,柱温为40℃。采用电喷雾正负离子同时扫描,多反应监测模式（MRM）进行质谱检测。结果:3种利尿剂在1.0~500.0 μg/L浓度范围内线性关系良好（r>0.996）;平均加标回收率67.3%~111.6%,方法检出限均为0.5 μg/kg,定量限均为1.0 μg/kg。结论:该方法简便、准确,可作为鸡肉和猪肉中利尿剂快速检测的方法。     

同位素稀释-超高效液相色谱-串联质谱法检测蜂蜜中泛酸含量

建立了同位素稀释-超高效液相色谱-串联质谱法（UPLC-MS/MS）检测蜂蜜中泛酸（维生素B5）的快速定量和确证方法。样品经0.1%氨水（V/V）提取,MAX固相萃取柱净化后,以0.1%甲酸乙腈-0.1%甲酸水为流动相梯度洗脱,使用HSS T3色谱柱进行分离,电喷雾正离子多反应监测（MRM）模式检测,同位素内标法定量。在优化条件下,泛酸在0.500～500 μg/L范围内线性良好,相关系数（R2）为0.999 6;方法检出限为1.0 μg/kg（S/N=3）,定量限为3.0 μg/kg（S/N=10）;回收率在98.3%～98.7%之间,相对标准偏差（RSD）为2.4%～3.1%。通过市售蜂蜜样品测试表明,该方法操作简单、检测结果准确,可用于蜂蜜中泛酸的快速检测。     

液相色谱法快速测定鸡肉中氧氟沙星手性对映体残留量

建立了鸡肉样品中氧氟沙星对映体液相色谱荧光检测(liquid chromatography fluorescence detector,LC-FLD)残留量快速分析方法。鸡肉样品经磷酸盐缓冲液提取后,用C18固相萃取小柱净化,洗脱液吹干后用流动相复溶即可进行液相色谱分析。分析时采用LeapsilTM C18色谱柱,以水相(含2 mmol/L硫酸铜和2.5 mmol/L异亮氨酸,pH3.5)和甲醇作为流动相进行梯度分析,荧光检测器检测,其中激发波长为297 nm,发射波长为487 nm,外标法定量。本方法在5.0、50、100μg/kg和150μg/kg 4个添加水平下,左氧氟沙星对映体平均添加回收率在75.5%～86.1%之间,批内变异系数在1.97%～4.42%之间,批间变异系数在3.02%～6.02%之间;右氧氟沙星对映体平均添加回收率在77.3%～84.9%之间,批内变异系数在2.15%～4.21%之间,批间变异系数在3.87%～5.84%之间。方法对两种对映体的检测限均为1.5μg/kg,定量限均为5.0μg/kg。     

多壁碳纳米管小柱-液质联用法测定鸡肉中兽药残留方法的研究

本实验建立了鸡肉中喹诺酮类、磺胺类、氯霉素类、四环素类兽药残留的液相色谱-串联质谱快速测定方法.研究了鸡肉中4类兽药残留的提取、净化前处理条件,试样用2.5％甲酸乙腈溶液提取,滤过型多壁碳纳米管小柱净化,Accucore VDX色谱柱梯度分离,三重四极杆质谱测定,基质标准曲线法定量.同时以电喷雾离子源正模式和负模式扫描...