高效液相色谱-串联质谱法测定动物源性食品中矮壮素残留

建立了高效液相色谱-串联质谱测定动物源性食品中矮壮素残留的分析方法。样品经含1%(v/v)乙酸的乙腈溶液提取、正己烷脱脂、阳离子固相萃取柱(PCX)净化,采用Venusil MP C18(2)色谱柱(150 mm×2.1 mm, 3μm)分离,以乙腈和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱,采用电喷雾电离、正离子模式扫描,多反应监测模式(MRM)检测,基质匹配标准曲线内标法定量。结果表明:矮壮素在0.200～500μg/L范围内呈良好线性,相关系数(r²)均不低于0.999 3,方法的定量限为0.500μg/kg;以猪肉、牛肉、羊肉、鸡肉、鸡蛋、猪肾、牛肝、羊肾、鸡肝、牛奶为基质,矮壮素的平均加标回收率为93.4%～101%,相对标准偏差为2.3%～8.0%。该方法基质干扰小,灵敏度高,准确可靠,适用于动物源性食品中矮壮素残留的定量检测。     

高效液相色谱-串联质谱法同时测定动物源性食品中35种兽药残留量

提出了高效液相色谱-串联质谱法同时测定动物源性食品中35种兽药残留量的方法。样品经含1%(体积分数)乙酸的乙腈提取,QuEChERS方法净化,所得净化液以Zobax Eclipse Plus C18色谱柱为分离柱,以不同体积比的0.1%甲酸(体积分数)溶液和乙腈混合液为流动相进行梯度洗脱,采用电喷雾正离子源和多反应监测模式检测。35种化合物的质量分数均在1~50μg·kg-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.02~1.07μg·kg-1之间,测定下限(10S/N)在0.08~3.58μg·kg-1之间。以空白样品为基体进行加标回收试验,所得回收率在45.6%~121%之间,相对标准偏差(n=6)在2.4%~24%之间。     

超高效液相色谱-串联质谱法测定动物源性食品中的磺胺增效剂

建立了一种超高效液相色谱-串联质谱（UPLC-MS/MS）测定多种基质（鸡肉、鱼肉、鸡肝、鸡蛋和牛奶）中三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶的分析方法。样品用甲酸-乙腈（1：9,v/v）溶液提取,正己烷除脂净化,Acquity UPLC BEH C18柱（50 mm×2.1 mm,1.7 μm）分离,以甲醇和5 mmol/L醋酸铵（含0.1%（v/v）甲酸）作为流动相进行梯度洗脱,电喷雾正离子（ESI⁺）模式电离,多反应监测（MRM）模式检测。考察了3种提取溶液的提取效率,优化了净化条件和浓缩条件,并对流动相、柱温和固相萃取柱进行了优化。结果表明：三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶在1.25~30.0 μg/L范围内线性关系良好（r≥0.99）。方法的定量限（S/N=10）为5.0 μg/kg,在5.0、10.0、20.0 μg/kg的添加浓度的回收率为61.2%~108.5%,相对标准偏差（RSD,n=6）为1.1%~9.8%。该方法快速、灵敏、准确,适合于多种基质中磺胺增效剂的测定。     

QuEChERS-高效液相色谱-串联质谱法测定动物源性食品中3种镇静剂残留

建立了QuEChERS-高效液相色谱-串联质谱(HPLC-MS/MS)同时测定猪肉、鱼肉、肝脏和肾脏中氯丙嗪、地西泮和安眠酮残留量的分析方法。样品用无水Na_2SO_4脱水、乙酸乙酯提取和C_(18)、N-丙基乙二胺(PSA)和氨基填料(NH2填料)净化,使用一种特殊的C_(18)色谱柱Atlantis T3,以5 mmol/L甲酸溶液和乙腈溶液为流动相进行梯度洗脱。在正离子电离多反应监测(MRM)模式下,采用同位素内标法进行定量分析。3种镇静剂在0.2~5.0μg/L范围内线性关系良好。3种镇静剂在4类基质中3个水平(0.5、1和5μg/kg)下的加标回收率为92.5%~117.8%,相对标准偏差(RSD)为0.7%~11.6%(n=6)。该法高效快捷,灵敏度高,基质适应范围广,适用于大批量样品的快速分析。     

同位素内标-液相色谱-串联质谱法测定动物源性食品中氯霉素残留

加入氯霉素同位素内标的动物源性样品(龙虾、肠衣)经乙酸乙酯提取浓缩、正己烷去脂后,采用液-液萃取,水相经0.45μm滤膜过滤后,用液相色谱-串联质谱定量.在0.1、0.2,0.3μg/kg3个浓度水平上进行添加回收试验.回收率为71.8%～90.0%,检出限为0.05μg/kg.该法简化了前处理操作步骤,缩短了检测时间...     

超高效液相色谱-串联质谱法对动物源性食品中13种β-内酰胺类药物残留的检测

建立了动物源性食品中青霉素G、青霉素V、阿莫西林、羧苄西林、氨苄西林、苯唑西林、氯唑西林、萘夫西林、头孢喹肟、头孢氨苄、头孢拉定、头孢唑啉和头孢哌酮13种β-内酰胺类药物残留检测的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法.样品经水和乙腈提取后,用正己烷去除脂肪,再用C18固相萃取柱净化,浓缩后用BEH C18色谱柱(50 mm×2.1 mm,1.7 μm)分离 ,以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测.结果表明:在5 ～500 μg/L的基质匹配标准溶液内13种β-内酰胺类药物均有良好的线性关系,相关系数(r)均大于0.998;样品中13种β-内酰胺类药物的检出限(LOD)均为1 ng/g,定量下限(LOQ)均为2 ng/g;在5 ～50 ng/g的加标范围内13种β-内酰胺类药物的平均回收率为79% ～99%,相对标准偏差(RSD)小于13.5%.     

液相色谱串联质谱法测定动物源性食品中硝呋烯腙的残留量

利用液相色谱-串联质谱(LC-ESI-MS/MS)测定动物源性食品中的硝呋烯腙残留量。通过实验,对样品前处理及仪器检测条件进行了优化。样品经提取和固相萃取净化后,采用HPLC-ESI-MS/MS进行检测,在多反应监测模式(MRM)下,外标法定量。方法的检出限为2.0μg/kg,在1.0～100.0μg/L范围内线性关系良好(相关系数r>0.99),平均添加回收率为66%～82%。     

动物源性食品中磺胺类药物增效剂残留的高效液相色谱-串联质谱法测定

利用高效液相色谱-电喷雾串联质谱测定了蜂蜜、蜂王浆、鮰鱼、鳗鱼、猪肉、猪肾、猪肝、鸡肉、牛肉和牛奶中的三甲氧苄氨嘧啶、二甲氧苄氨嘧啶和奥美普林3种磺胺类药物增效剂.除蜂王浆基质直接用10%三氯乙酸溶液提取外,其余基质均用10%三氯乙酸-乙腈(体积比7 : 3)混合溶液提取,提取溶液过阳离子交换固相萃取柱进行富集和净化.采用C18色谱柱,流动相为甲醇和0.1%甲酸溶液.选择1个母离子和2个子离子进行反应监测,对3种磺胺类药物增效剂残留进行定性,选择信号最强的子离子进行定量.在2 ～100 μg/L范围内,分析物的线性相关系数r>0.992.通过实际样品添加回收实验,所有基质定量下限为5.0 μg/kg,3个添加水平的回收率为63% ～89%,相对标准偏差为3.2% ～6.9%.     

动物源食品中6种甲状腺抑制剂残留的超高效液相色谱-串联质谱法检测

建立了动物源食品中2-硫脲嘧啶、6-甲基-2-硫脲嘧啶、6-丙基-2-硫脲嘧啶、6-苯基-2-硫脲嘧啶、2-巯基-1-甲基咪唑和2-巯基苯并咪唑6种甲状腺抑制剂残留检测的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。以BEHC18柱(50mm×2.1mm,1.7μm)为色谱柱,乙腈(含0.1%甲酸)-0.1%甲酸水溶液为流动相,梯度洗脱;柱温为30℃,流速为0.3mL/min,进样量为10μL。质谱条件为:电喷雾离子源(ESI+),多反应监测(MRM)模式。结果表明:6种药物在5～500μg/L质量浓度范围内呈良好的线性关系,相关系数r2均大于0.996;方法检出限为2μg/kg,定量下限为5μg/kg;在10、25、100μg/kg3个添加水平下,方法的平均回收率为60%～107%,批内、批间RSD均小于16%。     

超高效液相色谱-串联质谱法检测动物源性食品中残留的9种β-受体激动剂

建立了动物源性食品中特布他林、西马特罗、沙丁胺醇、非诺特罗、氯丙那林、莱克多巴胺、克仑特罗、妥布特罗和喷布特罗等9种β-受体激动剂残留检测的超高效液相色谱-串联质谱方法。样品经酶解后,用高氯酸去除蛋白质等杂质,调节上清液的pH值后,分别用乙酸乙酯和叔丁基甲醚进行萃取,再用MCX固相萃取柱净化,然后用Waters Acquity UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7 μm)分离,以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相进行梯度洗脱,外标法定量。结果表明:9种β-受体激动剂在0.25～5 μg/kg的空白添加浓度范围内呈良好的线性关系,相关系数(r)均大于0.990;特布他林等8种药物的检出限为0.1 μg/kg,定量限为0.25 μg/kg;喷布特罗的检出限为0.25 μg/kg,定量限为0.5 μg/kg。从0.5,1和2 μg/kg共3个添加浓度的检测结果可以看出,9种药物的平均回收率为87.1%～108.6%,批内、批间相对标准偏差(RSD)均小于20%。该方法具有简便快捷、灵敏度高、定性准确等特点。     

高效液相色谱串联质谱法同时测定水产品中24种性激素

建立了同时测定24种性激素的高效液相色谱串联质谱法,包括:睾酮、甲基睾酮、诺龙、苯丙酸诺龙、群勃龙、康力龙、勃地酮、雄烯二酮、美雄酮、炔诺酮、乙酸甲孕酮、乙酸甲羟孕酮、乙酸氯地孕酮、17α羟基孕酮、21α羟基孕酮、甲羟孕酮、左炔诺孕酮、雌酮、雌二醇、雌三醇、炔雌醇、己烷雌酚、己烯雌酚、双烯雌酚。乙酸乙酯提取2次,硅胶柱净化。采用甲醇、水作为流动相,经过CAPCELLPAK C18色谱柱分离后,采用APCI离子源,外标法定量。方法定量限为0.5～2μg/kg,加标回收率为80%～102%,相对标准偏差为6%～10%。方法实现了3类性激素的同时定量及确证分析。     

高效液相色谱-电喷雾串联质谱法同时测定鸡肉中残留的磺胺类和氟喹诺酮类兽药

建立了一种同时测定鸡肉中两类共10种兽药(3种磺胺和7种氟喹诺酮类药物)残留量的高效液相色谱-电喷雾串联质谱方法(HPLC -ESI-MS2)。样品经2%醋酸-乙腈提取,正己烷脱脂,过ENVI-18固相萃取柱净化,经氮气吹干后,残余物用流动相定容到1 mL。以乙腈和 0.05%甲酸溶液作为流动相,采用梯度洗脱程序进行液相色谱分离,用质谱检测器进行定性和定量分析,并对10种药物的二级质谱碎裂方 式进行分析。10种药物在0.02～2.0 mg/L范围内线性良好,相关系数均大于0.9988。检出限(LOD)为1.10～6.85 μg/kg,定量限(LOQ) 为3.68～22.85 μg/kg,样品的平均加标回收率为68.9%～102.6%,相对标准偏差均小于8.6%(n=3)。实验结果表明,该方法灵敏度高,重 现性好,确证能力强,分析时间短,可满足动物源性食品中磺胺和氟喹诺酮类药物的残留分析。     

Simultaneous determination of 24 sulfonamide residues in meat by ultra-performance liquid chromatography tandem mass spectrometry

The present study used the liquid extraction pretreatment method and developed an ultra-performance liquid chromatography triple quadrupole tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of 24 kinds of sulfonamide residues in meat. The meat samples were homogenized, extracted and deproteinized by acetonitrile, defatted by n-hexane, and further liquid-liquid extracted by ethyl acetate. All of 24 sulfonamide residues were simultaneously separated and determined by UPLC-MS/MS within 15 min. The sulfonamide residues were monitored via the ESI(+) ionization method and quantified by six-channel multiple reaction monitoring (MRM). The calibrations were performed in sample matrixes by the isotope dilution method and the interference effect of sample matrixes on the ionization was effectively eliminated. Good linear relationship (R(2)=0.991-0.999) was observed within the concentration range of 0.2-50 microg/kg. Satisfied recoveries (67.8-113.9%) of all the sulfonamides were demonstrated in different standard-spiked levels except sulfanitran (SNT). The analytical category, separation speed, selectivity, sensitivity and repeatability of sulfonamides using UPLC-MS/MS were significantly improved compared to other analytical methods. Quantitative results of 240 meat samples demonstrated that the present method has a convenient operation and good practicability, which can be applied to the quantitative analysis of a large number of samples.     

Simultaneous determination of 16 sulfonamides in honey by liquid chromatography/tandem mass spectrometry

A method is described for the determination of 16 sulfonamides in honey. Samples are dissolved in phosphoric acid solution (pH2), cleaned up with 2 solid-phase extraction (SPE) cartridges, an aromatic sulfonic cation-exchange cartridge and an Oasis HLB SPE cartridge, and analyzed both qualitatively and quantitatively by liquid chromatography/tandem mass spectrometry (LC/MS/MS) under the selected conditions. Without exception, calibration curves were linear (r = > 0.995), when sulfamethizole was between 1.0 and 25.0 microg/kg; sulfacetamide, sulfapyridine, sulfadiazine, sulfachloropyridazine, sulfamethoxazole, sulfamerazine, sulfisoxazole, sulfamonomethoxine, and sulfadoxine were between 2.0 and 50.0 microg/kg; sulfamethoxypyridazine, sulfadimethoxine, and sulfathiazole were between 4.0 and 100.0 microg/kg; sulfamethazine and sulfameter were between 8.0 and 200.0 microg/kg; and sulfaphenazole was between 12.0 and 300.0 microg/kg. Average recoveries at 4 fortification levels in the range of 1.0-300 microg/kg in honey were 70.9-102.5%, and relative standard deviations were 2.02-11.52%. The limits of quantitation for the 16 sulfonamides were between 1.0 and 12.0 microg/kg, with the LC/MS/MS method.     

UHPLC-MS/MS法快速测定水产品中17种磺胺和喹诺酮类药物

建立了UHPLC-MS/MS法测定水产品中10种磺胺类(SAs)和7种喹诺酮类(QNs)药物残留的分析方法。样品用200 g/L盐酸羟胺-乙腈溶液提取,以乙酸铵溶液和乙腈为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测模式检测,同时对水产品中10种SAs和7种QNs进行定量和定性。在0.25～4.0μg/kg和0.10～2.0μg/kg范围内两类药物的线性良好(r2>0.99);平均回收率为均为80%～120%,RSD为7.4%～14%;10种磺胺药物的检测限(LOD)均为5.0μg/kg,7种喹诺酮药物检测限(LOD)均为2.0μg/kg。该方法适合水产品中这两类药物残留的确证和定量测定。     

HPLC-MS/MS同时测定水产品中喹烯酮、喹乙醇和5种大环内酯类抗生素残留

建立了水产品中喹烯酮、喹乙醇和5种大环内酯类抗生素同时测定的高效液相色谱串联质谱法。向样品中加入无水硫酸钠,以乙酸乙酯-乙腈的混合溶液为提取剂,用正己烷净化。以乙腈-10 mmol/L甲酸铵溶液为流动相,流速为0.3 mL/min,以Hypersil GOLD为色谱分离柱,用配有电喷雾离子源的三重四极杆质谱进行定性定量分析。在1～1000 ng/mL范围内,7种药物呈良好线性关系。在鲫鱼、南美白对虾和甲鱼空白肌肉中添加水平为2～10μg/kg时,该方法的回收率为67.52%～108.89%,相对标准偏差为4.2%～14%,方法检测限为1μg/kg,定量限为2μg/kg。方法适用于同时测定水产品中喹烯酮、喹乙醇和5种大环内酯类药物的残留量。     

Rapid determination of quinolones in cosmetic products by ultra high performance liquid chromatography with tandem mass spectrometry

This study developed an improved analytical method for the simultaneous quantification of 13 quinolones in cosmetics by ultra high performance liquid chromatography combined with ESI triple quadrupole MS/MS under the multiple reaction monitoring mode. The analytes were extracted and purified by using an SPE cartridge. The limits of quantification ranged from 0.03 to 3.02 μg/kg. The precision for determining the quinolones was <19.39%. The proposed method was successfully developed for the determination of quinolones in real cosmetic samples.     

高效液相色谱-串联质谱法测定动物源食品中粘杆菌素、多粘菌素B的残留量

建立了动物源食品中粘杆菌素和多粘菌素B残留的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品用V(10%三氯乙酸水溶液):V(乙腈)=30:70提取,Oasis WCX SPE柱净化,LC-MS/MS电喷雾正离子多反应监测模式(ESI+-MRM)检测。分析物在0～250μg/kg的浓度范围内呈良好线性,线性相关系数>0.995。方法的定量限为10μg/kg。方法在三个添加水平的平均回收率在71.6%～78.9%之间,相对标准偏差在6.2%～12%之间。方法适用于动物源食品中粘杆菌素和多粘菌素B的定量及确证检测。     

Simultaneous determination of antiviral drugs in chicken tissues by ultra high performance liquid chromatography with tandem mass spectrometry

An ultra high performance liquid chromatography with tandem mass spectrometry method was established for the rapid and simultaneous analysis of seven antiviral drugs, amantadine, rimantadine, memantine, moroxydine, imiquimod, oseltamivir, and acyclovir, in chicken liver, muscle, and egg. Homogenized samples were extracted with trichloroacetic acid and acetonitrile solutions and then purified by cation‐exchange solid‐phase extraction. The target drugs were analyzed by liquid chromatography with a UPLC BEH Amide column (2.1 mm × 100 mm, 1.7 μm) coupled with a tandem mass spectrometer operating in the positive multiple‐reaction mode. A perfectly linear relationship was obtained within the concentration ranges of 0.5–20 μg/L for acyclovir and 0.1–10 μg/L for the other six antiviral drugs. The average recoveries of the seven antiviral drugs using four addition levels in chicken liver, muscle, and eggs were 82.67–90.10, 82.30–92.27, and 81.98–93.77%, respectively, and the acceptable coefficients of variation were 5.18–9.88, 4.84–11.2, and 42.8–9.95%, respectively. The detection limits and detection capabilities of the analysis method for the seven antiviral drugs were in the ranges of 0.04–0.64 and 0.11–0.78 μg/kg, respectively. Additionally, an inter‐laboratory study among five laboratories further validated the method.     

高效液相色谱-串联质谱法同时测定食品中五种黄色化工染料

采用高效液相色谱-串联质谱法(HPLC-MS/MS)建立了食品中非法添加的碱性橙、碱性嫩黄、酸性橙I、酸性橙II和酸性黄36这5种黄色工业染料的定量定性分析方法。使用Agilent ODS C18分离柱(50 mm×2.0 mm, 1.8 μm),以5 mmol/L乙酸铵水溶液(0.1%甲酸)-乙腈(3:2, v/v)为流动相,流速为0.3 mL/min。采用电喷雾离子化源,以多反应监测(MRM)方式分别在正、负离子模式下进行检测。在最佳检测条件下,得到了较宽的线性范围和较低的定量检出限。碱性橙和碱性嫩黄的线性范围均为5.0～80.0 mg/L;酸性橙I、酸性橙II及酸性黄36的线性范围均为10.0～160.0 μg/L。食品中碱性橙、碱性嫩黄、酸性橙I、酸性橙II及酸性黄36的定量限分别为20、20、40、40、40 ng/g。该方法重现性较好,保留时间和峰面积的相对标准偏差分别不大于0.50%和2.14%。本研究还测定了鸡肉、豆制品和黄鱼中添加的5种化工染料,回收率在79.8%~95.2%之间,结果令人满意。