液相色谱-串联质谱法测定小麦、麦秸和土壤中氟唑磺隆及其代谢物残留

An analytical method was developed to measure the residues of Flucarbazone-sodium and its Metabolites in wheat grain, straw, and soil by HPLC-MS/MS. The lowest level of method validation (LLMV) is 0.01 mg•kg^－1 for Flucarbazone-sodium and its Metabolites in straw and soil, and 0.005 mg•kg^－1 in wheat grain. The average fortified recoveries are between 74% and 103% with a relative standard deviation (RSD) between 3.4% and 16.3%.     

液相色谱-串联质谱法测定动物组织中1，2-二苯乙烯类药物残留的研究

建立了固相萃取-液相色谱-串联质谱法同时测定动物组织中3种1,2-二苯乙烯类药物（包括己二烯雌酚、己烯雌酚、己烷雌酚）残留量的方法。试样中的药物经甲醇超声提取后,过HLB固相萃取柱净化、氮吹至干,用流动相溶解后进行液相色谱 串联质谱法测定,以D₈-己烯雌酚为内标进行定量分析。方法的最低检出限为0.2 μg•kg^-1,定量限均为0.5 μg•kg^-1;在1.0～100 μg•L^-1 范围内线性良好;加标浓度在0.5～10 μg•kg^-1 范围内,动物组织中己二烯雌酚、己烯雌酚、己烷雌酚的回收率在78.8％～110.9％,批内相对标准偏差小于或等于8.0％,能满足相关法规要求。     

LC-MS/MS法定量测定人血浆中TF及其代谢产物M1，M2

A sensitive liquid chromatography-electrospray ionization-tandem mass spectrometric(LC-MS/MS) method for the simultaneous determination of TF and its metabolites M1 and M2 in human plasma were developed and validated. The plasma TF, M1, M2 were extracted using a solid phase extraction(SPE), and the sample extract was injected onto the LC-MS/MS system. The limits of quantitation(LLOQ) for TF, M1, M2 are 1 ng•L^－1. This method allowes the reproducible and accurate quantification with the concentration range of 1-500 ng•L^－1. This method can be applied to the quantitation of TF, M1, M2 in human plasma.     

气相色谱-质谱法测定奶粉中的三聚氰胺

Melamine in milk power was determined by gas chromatography-mass spectrometer(GC/MS) made in china. The results show that the method has a good liner range between 0.005 mg•L^－1 and 2 mg•L^－1, R2 is 0.999 7. The limit of detection is 0.001 mg•L^－1, the quantitative detection limit is 0.02 mg•kg^－1. The recovery for melamine is in the range of 94％-102％. The method has good sensitivity, selectivity and repeatability, which has been applied to the determination of melamine in milk powder.     

GC/MS法测定人血清中角鲨烯与6种非胆固醇类固醇含量

Besides cholesterol, a few of squalene and non-cholesterol sterols exist in human serum, which include cholesterol synthesis precursors (e.g. desmosterol and lathosterol) and plant sterols (e.g. campesterol, stigmasterol, sitosterol and cholestanol). In present studies, squalene and cholesterol precursors could be considered as cholesterol synthesis markers, which reflect synthesis efficiency of cholesterol, while plant sterols are considered as cholesterol absorption markers which reflect cholesterol absorption efficiency. Because of the similar molecule structure among cholesterol and non-cholesterol sterols, and the less content of non-cholesterol sterols, the present method, such as radioactive isotope, high-performance liquid chromatography (HPLC), and gas chromatography (GC), have some difficulties in the separation and quantification of non-cholesterol sterols. In our studies, the method of sample preparation was improved, and the chemical derivation process was also optimized, and GC/MS were used in the quantitative determination of cholesterol and non-cholesterol sterols. Compared to GC method, our method has a better resolution and repeatability, and the accuracy is also good, so it is feasible to use the method in analysis for clinical individual difference of cholesterol metabolism. Serum of 30 patients of hyperlipemia were determined by our method, and the mean values of squalene and sterols are squalene 0.18 mg•dL^－1, cholestanol 0.69 mg•dL^－1, desmosterol 0.03 mg•dL^－1, lathosterol 0.31 mg•dL^－1, campesterol 0.27 mg•dL^－1, stigmasterol 0.05 mg•dL－1 and sitosterol 0.39 mg•dL^－1. The total content of squalene and non-cholesterol sterols is 1.53 mg•dL^－1, which is 0.89% of cholesterol. Linear regression analysis is made between all kinds of sterols. Cholesterol has positive correlation with all 6 non-cholesterol sterols. Whereas, the positive correlations with cholestanol and stigmasterol are not significant probably due to the serum quantity is not enough. More serum data will need to obtain more representative results.     

分散型固相萃取-气相色谱串联质谱法测定食品中8种芳氧苯氧丙酸酯类除草剂的残留量

建立了大豆、绿茶、大米、胡萝卜、菠菜、豌豆、大蒜、草莓、蜂蜜、猪肉、鱼肉、鸡蛋等12种食品中8种芳氧苯氧丙酸酯类除草剂残留量的分散型固相萃取-气相色谱串联质谱(DSPE-GC-MS/MS)分析方法。样品由含1%冰醋酸的正己烷的饱和乙腈溶液提取,分散型固相萃取法净化,采用气相色谱-串联质谱分时段反应离子监测技术进行测定,外标法定量。所有农药在10~1 000μg.L-1范围内线性良好;方法定量限(LOQ)均低于10μg.kg-1;在10、20、40μg.kg-1三个添加水平下,大豆等12种代表性基质中所有农药的平均回收率均处于70%~120%之间,RSD≤13%;该方法选择性较好,不仅能够用于多种食品基质的残留检测,而且还能较好地解决本底成分相当复杂的大蒜基质极易出现的干扰问题。     

高效液相色谱-串联质谱法在他克莫司临床血药浓度监测中的应用

建立高效液相色谱-质谱联用法监测人全血中他克莫司浓度。选用Shim-pack VP-ODS色谱柱，以甲醇10 mmol•L^-1乙酸铵为流动相，采用梯度洗脱进行分离，样品用乙腈进行蛋白沉淀后进样，用3200Qtrap型质谱仪的多重反应监测（MRM）扫描方式进行检测。他克莫司的线性范围为0.5~50.0 μg•L^-1，定量下限和最低检测限分别为0.5、0.1 μg•L^-1。准确度与精密度结果显示方法日间、日内变异均小于6.8%，相对偏差为-2.99%~2.23%，方法提取回收率均接近100.0%，稳定性较好。该方法快速、灵敏、专属性强、重现性高，适用于他克莫司治疗药物监测（TDM）工作。     

LC-MS/MS法定量测定人血浆中CPRC-127血药浓度

A sensitive liquid chromatography-electrospray ionization-tandem mass spectrometric(LC-MS/MS) method for the determination of CPRC-127 in human plasma was developed and validated. The plasma was extracted using a liquid-liquid phase extraction(LLE), and the sample extract was injected onto the LC-MS/MS system. The limit of quantitation(LLOQ) for CPRC-127 is 0.5 μg•L^－1. This method allows the reproducible and accurate quantification with the concentration range of 0.5-1 000 μg•L^－1. This method can be applied to the quantitation of CPRC-127 in human plasma.     

液相色谱-串联质谱法确证人尿中的利他林及其主要代谢物

建立了固相萃取-液相色谱-串联质谱法同时确证人尿中的利他林及其主要代谢物利他林酸的方法。尿样中的药物经反相C₁₈固相萃取柱净化、氮气吹至干,以甲睾为内标,用流动相溶解后进行液相色谱-串联质谱法测定。该方法的最低检出限为5 μg•L^-1;利他林和利他林酸的回收率分别为80.6%和68.4%;批内和批间的相对标准偏差小于6.0%,能满足国际反兴奋剂机构(WADA)对其最低检测能力500 μg•L^-1的要求。     

LC-MS/MS法结合谱库检索测定猪组织中三聚氰胺及其同系物

采用MRM→IDA→EPI→谱库检索模式建立了猪组织中三聚氰胺及其同系物的液相色谱-电喷雾串联质谱多残留检测方法,结合谱库检索功能同时实现了定性定量分析。组织样品经2%三氯乙酸、10%乙酸铅和乙腈混合溶液提取,Sepucol ENVI-CARB柱净化,三聚氰胺及其同系物的线性范围为10~5 000μg.kg-1,线性关系良好(r0.99);在10~100μg.kg-1添加水平范围内,平均回收率为94.2%~99.9%、相对标准偏差为3.8%~7.5%、方法检出限为2μg.kg-1。