采用超高效液相色谱-串联质谱技术对贵州省3个产地的蜂糖李果实初生代谢物进行代谢组学研究,通过主成分分析、正交偏最小二乘判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)等多元统计分析和代谢途径分析,...采用超高效液相色谱-串联质谱技术对贵州省3个产地的蜂糖李果实初生代谢物进行代谢组学研究,通过主成分分析、正交偏最小二乘判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)等多元统计分析和代谢途径分析,探讨产地对蜂糖李初生代谢产物的影响。实验共鉴定出307种代谢物,分析发现产地对蜂糖李代谢物的种类和含量均有影响。良田蜂糖李相比六马蜂糖李存在13种差异代谢物,惠水蜂糖李相比六马蜂糖李、良田蜂糖李都存在49种差异代谢物。同时OPLS-DA结果表明,不同产地蜂糖李区分明显,均有显著样本聚集区,说明产地对蜂糖李初生代谢的影响很大。代谢通路分析发现,不同产地间蜂糖李初生代谢差异机制主要在于氨基酸类物质的代谢,对氨基酸类物质的影响最为显著。本研究可为蜂糖李产地鉴别提供理论依据,为蜂糖李产地溯源提供一定参考。展开更多
The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tande...The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining catecholamines and metanephrines in urine to replace an existing liquid chromatographic method using electrochemical detection.Urine samples were prepared using Oasis weak-cation-exchange cartridges.The eluate was analyzed on an Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column in 3 min.Adrenaline,noradrenaline,dopamine,metanephrine,normetanephrine,and their deuterated internal standards were monitored in positive electrospray ionization mode by multiple reaction monitoring(MRM).No evidence of ion suppression was observed.The assay was linear up to 5μmol/L for adrenaline,5μmol/L for noradrenaline,6.1μmol/L for dopamine,5.6μmol/L for metanephrine,and 34.6μmol/L for normetanephrine,with lower limits of quantification of 5,5,12,6 and 7nmol/L,respectively.The intra-day and inter-day precisions for all analytes ranged from 0.59%to 4.64%and1.98%to 4.80%,respectively.External quality assurance samples were assayed and showed excellent agreement with the target values.This simple method provides an improved assay for determining urine catecholamines and metanephrines.展开更多
An accurate and sensitive method for the simultaneous determination of gibberellic acid（GA3）, gibberellin A4（GA4） and gibberellin A7（GA7） residues in tomato paste was developed by coupling solid phase extraction...An accurate and sensitive method for the simultaneous determination of gibberellic acid（GA3）, gibberellin A4（GA4） and gibberellin A7（GA7） residues in tomato paste was developed by coupling solid phase extraction to high performance liquid chromatography-tandem mass spectrometry（LC-MS/MS） with electrospray ionization based stable isotope dilution analysis（SIDA）. The isotope labeled internal standard can compensate for the losses during the extraction and cleanup steps and for discrimination due to ion suppression. After extraction from methanol, hydrophile lipophilic balance（HLB） solid phase extraction（SPE） column was tested for the capacity of the cleanup of the tomato paste in compared with C18 SPE column which is the common way to the detection of GAs, and the former gained better result. Spiked experiments were performed in the non-contaminated tomato pastes and the recoveries of GA3, GA4 and GA7 were 42.6%―75.0% in external standard method（ESM） and 91.1%―103.8% in internal standard method（ISM） respectively. The validities of this method were investigated and good analytical performance for the three GAs was obtained, including low limits of method detection（2 ng/g for GA3 and GA4, 0.3 ng/g for GA7）, excellent linear dynamic ranges（5―500 ng/g for GA3 and GA4, 1―100 ng/g for GA7） and good relative standard deviation ranges（4.8%―9.4% for the intra-day test and 3.5%―11.9% for the inter-day test）.展开更多
Over the past decade, the use of hair specimens for the long-term detection of the alcohol biomarker ethyl glucuronide has been increasing in popularity and usage. We evaluated the usefulness of fingernail clippings a...Over the past decade, the use of hair specimens for the long-term detection of the alcohol biomarker ethyl glucuronide has been increasing in popularity and usage. We evaluated the usefulness of fingernail clippings as a suitable alterna-tive to hair for ethyl glucuronide detection. A liquid chromatography-tandem mass spectrometry method for the detection of ethyl glucuronide in fingernail clippings was fully validated and used to analyze the hair and/or fingernail specimens of 606 college-aged study participants. The limit of detection was 2 pg/mg, the limit of quantitation was 8 pg/mg and the method was linear from 8 to 2000 pg/mg. Intra- and inter-assay imprecision studies at three different concentrations (20, 40, 200 pg/mg) were all within 7.8% and all intra- and inter-assay bias studies at these levels were within 115.1% of target concentration. Ethyl glucuronide levels in fingernail (mean = 29.1 ± 55.6 pg/mg) were higher than ethyl glucuronide levels in hair (mean = 9.48 ± 22.3 pg/mg) and a correlation of the matched pairs was observed (r = 0.552, P < 0.01, n = 529). Evaluating each gender separately revealed that the correlation of male fingernail to male hair was large and significant (r = 0.782, P < 0.01, n = 195) while female hair to female fingernail was small yet sig-nificant (r = 0.249, P < 0.01, n = 334). The study results demonstrated that fingernail may be a suitable alternative to hair for ethyl glucuronide detection and may be the preferred sample type due to the lack of a gender bias.展开更多
A simple, rapid and sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） for the determination of glycyrrhetic acid in human plasma with ginsenoside Rh2 as internal standard was developed and validated...A simple, rapid and sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） for the determination of glycyrrhetic acid in human plasma with ginsenoside Rh2 as internal standard was developed and validated. The plasma samples were prepared via liquid-liquid extraction with ethyl acetate. Chromatographic separation was accomplished on a Venusil MP-C18（50 mm×2.1 mm, 5 μm i.d.） column at 25 °C. The mobile phase consisted of acetonitrile/5 mmol？L-1 ammonium acetate（10：90, volume ratio） at a flow rate of 0.4 mL/min. Negative electrospray ionization was utilized as the ionization source. Glycyrrhetic acid and internal standard were determined via the mutiple reaction monitoring of precursor→production ion transitions at m/z 469→425, 409 and m/z 621→161, respectively. Each sample was chromatographed within 2.5 min. The lower limit of quantification was 0.50 ng/mL for 200 μL of plasma sample and the linear range was from 0.50 ng/mL to 800 ng/mL. The intra- and inter-day precisions were less than 8.76% in terms of relative standard deviation（RSD）, and the accuracy was within a range of -3.25%-1.32% in terms of relative error（RE）. The method was successfully applied to the pharmacokinetic studies of glycyrrhetic acid in healthy male Chinese volunteers after a single oral administration of 75 mg of glycyrrhizin.展开更多
建立人参中30种农药残留的快速样品处理,联合液相色谱-串联质谱(quick,easy,cheap,effective,rugged and safe/liquid chromatography tandem mass spectrometry,QuEChERS/LC-MS/MS)检测方法。通过对快速样品处理法(QuEChERS)的净化剂...建立人参中30种农药残留的快速样品处理,联合液相色谱-串联质谱(quick,easy,cheap,effective,rugged and safe/liquid chromatography tandem mass spectrometry,QuEChERS/LC-MS/MS)检测方法。通过对快速样品处理法(QuEChERS)的净化剂配比和LC-MS/MS质谱条件等优化,探究人参中30种农药多残留的最优测定方法。确定C18(100 mg)为净化剂,无水硫酸钠为提取盐包,30种农药多残留的回收率范围均在60%~120%,线性关系良好,相关系数均不低于0.99,变异系数范围均小于15%,测定低限均不大于2020版《中国药典》规定的定量限。该方法适用于人参中30种农药多残留的测定。展开更多
建立并验证了一种基于QuEChERS前处理的超高效液相色谱串联质谱法(ULTRA Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS/MS)快速测定鸡蛋中6种磺胺类化合物和甲氧苄啶的分析方法。样品经1%乙酸乙腈超声提取,加NH...建立并验证了一种基于QuEChERS前处理的超高效液相色谱串联质谱法(ULTRA Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS/MS)快速测定鸡蛋中6种磺胺类化合物和甲氧苄啶的分析方法。样品经1%乙酸乙腈超声提取,加NH_(4)Cl和NaCl盐析分层后,使用新型吸附剂Zep^(+)、MWNTs进行净化。提取物经C_(18)色谱柱分离,采用电喷雾电离,多反应监测模式进行测定。结果表明6种磺胺化合物和甲氧苄啶回收率在60.7%~119.0%,相对标准偏差在0.50%~14.00%,检出限(LODs)为5μg·kg^(-1),定量限(LOQs)为10μg·kg^(-1),改良的QuEChERS-LC-MS/MS方法极大地提高了磺胺多残留的检测效率,适用于鸡蛋中磺胺多残留的快速分析。展开更多
A high-performance liquid chromatography (HPLC) method has been developed for the determination of bemegride and its salts in cosmetics. A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) m...A high-performance liquid chromatography (HPLC) method has been developed for the determination of bemegride and its salts in cosmetics. A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was used for the verification of the analytical results. Cosmetic samples were ultrasonically extracted with methanol, centrifuged and filtered by microporous membrane filter prior to instrumental analysis. The chromatographic separation of the analytes was performed using a Symmetry C18 (4.6 mm × 250 mm, 5 μm) column. The quantitation was carried out by external standard method. The experimental results indicated that the limit of quantitation (LOQ) for bemegride and its salts was 0.5 mg/kg. The mean recoveries at three spiked levels ranged from 85.1% to 107.4% with the relative standard deviations (RSDs) between 3.7% and 9.3%. The suspected positive samples were subjected to further verification by HPLC-MS/ MS. The method is accurate, rapid, sensitive and can be used for the inspection of cosmetics.展开更多
提出了题示方法测定衢枳壳样品中黄曲霉毒素B1、B2、G1、G2和赭曲霉毒素A的含量。样品经过体积比79∶20∶1的乙腈-水-乙酸混合溶液超声提取,离心,上清液用p H 7.0磷酸盐缓冲液稀释,用复合免疫亲和柱净化,过滤,滤液中的目标物在XDB C18...提出了题示方法测定衢枳壳样品中黄曲霉毒素B1、B2、G1、G2和赭曲霉毒素A的含量。样品经过体积比79∶20∶1的乙腈-水-乙酸混合溶液超声提取,离心,上清液用p H 7.0磷酸盐缓冲液稀释,用复合免疫亲和柱净化,过滤,滤液中的目标物在XDB C18色谱柱上用不同体积比的体积比1∶9的甲醇-5 mmol·L^(-1)乙酸铵混合溶液和体积比9∶1的甲醇-5 mmol·L^(-1)乙酸铵混合溶液的混合溶液分离,电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式检测,同位素内标法定量。结果显示:5种真菌毒素与其同位素内标质量浓度比和对应的峰面积比在一定范围内呈线性关系,检出限为0.05~0.20μg·kg^(-1)。3个加标浓度水平下阴性样品中5种真菌毒素的回收率为82.7%~97.3%,测定值的相对标准偏差(n=6)为5.2%~12%。展开更多
对7种经典农药使用液相色谱串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测在6种常见蔬菜中的杀虫剂和杀菌剂残留。实验过程中,严格遵循GB 23200.121—2021标准,对6种蔬菜中的7种农药含量进行精确测定。通...对7种经典农药使用液相色谱串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测在6种常见蔬菜中的杀虫剂和杀菌剂残留。实验过程中,严格遵循GB 23200.121—2021标准,对6种蔬菜中的7种农药含量进行精确测定。通过分析基质和溶剂标准曲线的线性方程的斜率,从而判断它们对基质的作用。结果显示蔬菜中的农药残留量主要以基质减弱为主,其中在黄瓜、茄子和豇豆中,哒螨灵、甲氨基阿维菌素苯甲酸盐以及噻虫嗪都表现出了明显的基质效应。这意味着,在农药残留检测时,如果使用基质标准曲线进行定量测定可以得到更准确的结果。农药残留的精度受到基质效应的显著影响,所以降低和消除这种效应在维护食品安全方面起着关键作用。展开更多
过敏原的硝基化会引起其致敏潜能的增强,进而带来更大的致敏性健康风险.过敏原蛋白质通常含有多个酪氨酸硝基化位点,分析过敏原硝基化的位点选择性是探究硝基化对过敏原致敏性影响的重要基础.本文以尘螨过敏原为研究对象,建立了基于超...过敏原的硝基化会引起其致敏潜能的增强,进而带来更大的致敏性健康风险.过敏原蛋白质通常含有多个酪氨酸硝基化位点,分析过敏原硝基化的位点选择性是探究硝基化对过敏原致敏性影响的重要基础.本文以尘螨过敏原为研究对象,建立了基于超高效液相色谱-串联质谱(UPLC-MS/MS)同时定量分析3种尘螨过敏原(Der f 1、Der p 1和Der p 2)的13个酪氨酸位点硝基化程度的方法,并应用于分析3种尘螨过敏原在过氧亚硝酸盐硝基化作用下的位点选择性.结果表明,3种尘螨过敏原均发生了位点特异性的硝基化,Y195、Y37和Y92分别为Der f 1、Der p 1和Der p 2中反应活性最高的硝基化位点.尘螨过敏原位点选择性的硝基化表明,在评价硝基化尘螨过敏原的致敏性变化时应当考虑其位点特异性的硝基化状况.展开更多
文摘采用超高效液相色谱-串联质谱技术对贵州省3个产地的蜂糖李果实初生代谢物进行代谢组学研究,通过主成分分析、正交偏最小二乘判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)等多元统计分析和代谢途径分析,探讨产地对蜂糖李初生代谢产物的影响。实验共鉴定出307种代谢物,分析发现产地对蜂糖李代谢物的种类和含量均有影响。良田蜂糖李相比六马蜂糖李存在13种差异代谢物,惠水蜂糖李相比六马蜂糖李、良田蜂糖李都存在49种差异代谢物。同时OPLS-DA结果表明,不同产地蜂糖李区分明显,均有显著样本聚集区,说明产地对蜂糖李初生代谢的影响很大。代谢通路分析发现,不同产地间蜂糖李初生代谢差异机制主要在于氨基酸类物质的代谢,对氨基酸类物质的影响最为显著。本研究可为蜂糖李产地鉴别提供理论依据,为蜂糖李产地溯源提供一定参考。
文摘The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining catecholamines and metanephrines in urine to replace an existing liquid chromatographic method using electrochemical detection.Urine samples were prepared using Oasis weak-cation-exchange cartridges.The eluate was analyzed on an Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column in 3 min.Adrenaline,noradrenaline,dopamine,metanephrine,normetanephrine,and their deuterated internal standards were monitored in positive electrospray ionization mode by multiple reaction monitoring(MRM).No evidence of ion suppression was observed.The assay was linear up to 5μmol/L for adrenaline,5μmol/L for noradrenaline,6.1μmol/L for dopamine,5.6μmol/L for metanephrine,and 34.6μmol/L for normetanephrine,with lower limits of quantification of 5,5,12,6 and 7nmol/L,respectively.The intra-day and inter-day precisions for all analytes ranged from 0.59%to 4.64%and1.98%to 4.80%,respectively.External quality assurance samples were assayed and showed excellent agreement with the target values.This simple method provides an improved assay for determining urine catecholamines and metanephrines.
基金Supported by the Project of Chinese Academy of Inspection and Quanrantine(No.2010JK001)the Project of Xinjiang Entry-exit Inspection and Quarantine Bureau, China(No.2010XK0033)
文摘An accurate and sensitive method for the simultaneous determination of gibberellic acid（GA3）, gibberellin A4（GA4） and gibberellin A7（GA7） residues in tomato paste was developed by coupling solid phase extraction to high performance liquid chromatography-tandem mass spectrometry（LC-MS/MS） with electrospray ionization based stable isotope dilution analysis（SIDA）. The isotope labeled internal standard can compensate for the losses during the extraction and cleanup steps and for discrimination due to ion suppression. After extraction from methanol, hydrophile lipophilic balance（HLB） solid phase extraction（SPE） column was tested for the capacity of the cleanup of the tomato paste in compared with C18 SPE column which is the common way to the detection of GAs, and the former gained better result. Spiked experiments were performed in the non-contaminated tomato pastes and the recoveries of GA3, GA4 and GA7 were 42.6%―75.0% in external standard method（ESM） and 91.1%―103.8% in internal standard method（ISM） respectively. The validities of this method were investigated and good analytical performance for the three GAs was obtained, including low limits of method detection（2 ng/g for GA3 and GA4, 0.3 ng/g for GA7）, excellent linear dynamic ranges（5―500 ng/g for GA3 and GA4, 1―100 ng/g for GA7） and good relative standard deviation ranges（4.8%―9.4% for the intra-day test and 3.5%―11.9% for the inter-day test）.
文摘Over the past decade, the use of hair specimens for the long-term detection of the alcohol biomarker ethyl glucuronide has been increasing in popularity and usage. We evaluated the usefulness of fingernail clippings as a suitable alterna-tive to hair for ethyl glucuronide detection. A liquid chromatography-tandem mass spectrometry method for the detection of ethyl glucuronide in fingernail clippings was fully validated and used to analyze the hair and/or fingernail specimens of 606 college-aged study participants. The limit of detection was 2 pg/mg, the limit of quantitation was 8 pg/mg and the method was linear from 8 to 2000 pg/mg. Intra- and inter-assay imprecision studies at three different concentrations (20, 40, 200 pg/mg) were all within 7.8% and all intra- and inter-assay bias studies at these levels were within 115.1% of target concentration. Ethyl glucuronide levels in fingernail (mean = 29.1 ± 55.6 pg/mg) were higher than ethyl glucuronide levels in hair (mean = 9.48 ± 22.3 pg/mg) and a correlation of the matched pairs was observed (r = 0.552, P < 0.01, n = 529). Evaluating each gender separately revealed that the correlation of male fingernail to male hair was large and significant (r = 0.782, P < 0.01, n = 195) while female hair to female fingernail was small yet sig-nificant (r = 0.249, P < 0.01, n = 334). The study results demonstrated that fingernail may be a suitable alternative to hair for ethyl glucuronide detection and may be the preferred sample type due to the lack of a gender bias.
基金Supported by the Xinjiang Vurge Autonomous Region(China) Tackle Key Problems in Science and Technology and Plan of Emphasis Project(No.200733146-4)
文摘A simple, rapid and sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） for the determination of glycyrrhetic acid in human plasma with ginsenoside Rh2 as internal standard was developed and validated. The plasma samples were prepared via liquid-liquid extraction with ethyl acetate. Chromatographic separation was accomplished on a Venusil MP-C18（50 mm×2.1 mm, 5 μm i.d.） column at 25 °C. The mobile phase consisted of acetonitrile/5 mmol？L-1 ammonium acetate（10：90, volume ratio） at a flow rate of 0.4 mL/min. Negative electrospray ionization was utilized as the ionization source. Glycyrrhetic acid and internal standard were determined via the mutiple reaction monitoring of precursor→production ion transitions at m/z 469→425, 409 and m/z 621→161, respectively. Each sample was chromatographed within 2.5 min. The lower limit of quantification was 0.50 ng/mL for 200 μL of plasma sample and the linear range was from 0.50 ng/mL to 800 ng/mL. The intra- and inter-day precisions were less than 8.76% in terms of relative standard deviation（RSD）, and the accuracy was within a range of -3.25%-1.32% in terms of relative error（RE）. The method was successfully applied to the pharmacokinetic studies of glycyrrhetic acid in healthy male Chinese volunteers after a single oral administration of 75 mg of glycyrrhizin.
文摘建立人参中30种农药残留的快速样品处理,联合液相色谱-串联质谱(quick,easy,cheap,effective,rugged and safe/liquid chromatography tandem mass spectrometry,QuEChERS/LC-MS/MS)检测方法。通过对快速样品处理法(QuEChERS)的净化剂配比和LC-MS/MS质谱条件等优化,探究人参中30种农药多残留的最优测定方法。确定C18(100 mg)为净化剂,无水硫酸钠为提取盐包,30种农药多残留的回收率范围均在60%~120%,线性关系良好,相关系数均不低于0.99,变异系数范围均小于15%,测定低限均不大于2020版《中国药典》规定的定量限。该方法适用于人参中30种农药多残留的测定。
文摘建立并验证了一种基于QuEChERS前处理的超高效液相色谱串联质谱法(ULTRA Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS/MS)快速测定鸡蛋中6种磺胺类化合物和甲氧苄啶的分析方法。样品经1%乙酸乙腈超声提取,加NH_(4)Cl和NaCl盐析分层后,使用新型吸附剂Zep^(+)、MWNTs进行净化。提取物经C_(18)色谱柱分离,采用电喷雾电离,多反应监测模式进行测定。结果表明6种磺胺化合物和甲氧苄啶回收率在60.7%~119.0%,相对标准偏差在0.50%~14.00%,检出限(LODs)为5μg·kg^(-1),定量限(LOQs)为10μg·kg^(-1),改良的QuEChERS-LC-MS/MS方法极大地提高了磺胺多残留的检测效率,适用于鸡蛋中磺胺多残留的快速分析。
文摘A high-performance liquid chromatography (HPLC) method has been developed for the determination of bemegride and its salts in cosmetics. A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was used for the verification of the analytical results. Cosmetic samples were ultrasonically extracted with methanol, centrifuged and filtered by microporous membrane filter prior to instrumental analysis. The chromatographic separation of the analytes was performed using a Symmetry C18 (4.6 mm × 250 mm, 5 μm) column. The quantitation was carried out by external standard method. The experimental results indicated that the limit of quantitation (LOQ) for bemegride and its salts was 0.5 mg/kg. The mean recoveries at three spiked levels ranged from 85.1% to 107.4% with the relative standard deviations (RSDs) between 3.7% and 9.3%. The suspected positive samples were subjected to further verification by HPLC-MS/ MS. The method is accurate, rapid, sensitive and can be used for the inspection of cosmetics.
文摘对7种经典农药使用液相色谱串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测在6种常见蔬菜中的杀虫剂和杀菌剂残留。实验过程中,严格遵循GB 23200.121—2021标准,对6种蔬菜中的7种农药含量进行精确测定。通过分析基质和溶剂标准曲线的线性方程的斜率,从而判断它们对基质的作用。结果显示蔬菜中的农药残留量主要以基质减弱为主,其中在黄瓜、茄子和豇豆中,哒螨灵、甲氨基阿维菌素苯甲酸盐以及噻虫嗪都表现出了明显的基质效应。这意味着,在农药残留检测时,如果使用基质标准曲线进行定量测定可以得到更准确的结果。农药残留的精度受到基质效应的显著影响,所以降低和消除这种效应在维护食品安全方面起着关键作用。
文摘过敏原的硝基化会引起其致敏潜能的增强,进而带来更大的致敏性健康风险.过敏原蛋白质通常含有多个酪氨酸硝基化位点,分析过敏原硝基化的位点选择性是探究硝基化对过敏原致敏性影响的重要基础.本文以尘螨过敏原为研究对象,建立了基于超高效液相色谱-串联质谱(UPLC-MS/MS)同时定量分析3种尘螨过敏原(Der f 1、Der p 1和Der p 2)的13个酪氨酸位点硝基化程度的方法,并应用于分析3种尘螨过敏原在过氧亚硝酸盐硝基化作用下的位点选择性.结果表明,3种尘螨过敏原均发生了位点特异性的硝基化,Y195、Y37和Y92分别为Der f 1、Der p 1和Der p 2中反应活性最高的硝基化位点.尘螨过敏原位点选择性的硝基化表明,在评价硝基化尘螨过敏原的致敏性变化时应当考虑其位点特异性的硝基化状况.
