高效液相色谱-串联质谱法测定鸡蛋中三聚氰胺残留

An high-performance liquid chromatographic method with tandem mass spectrometry(HPLC-MS/MS) was developed for the determination of melamine residues in egg. In the method, the melamine residue was extracted with V(1% Trichloroacetic acid):V(methanol)＝1:1, cleaned-up with PCX solid phase extraction column, and concentrated to dry under nitrogen and redissolved in 1 mL dissolving solution. The solution was separated on a RP-HPLC column, and detected by HPLC-MS/MS with positive electrospray ionization(ESI＋) in multiple reaction monitoring(MRM) mode. Quantitation was carried out using an external standard method. The standard curves for all compounds are linear over the concentration range of 20-400 μg kg^－1 with correlation coefficients(r2) of 0.998 5. The recoveries of melamine from egg samples spiked with the concentration levels at 50, 100, 200 μg kg^－1 are range of 87.0%, 96.8%, 94.4%. The limits of detection for the method are 3 μg kg^－1. The limits of quantification for the method are 10 μg kg^－1. The results show that the established method is of simplicity, rapidity, high sensitivity, good reproducibility and better selectivity. The method is quite fit for identification and determination of melamine in egg.     

应用液相色谱-质谱联用技术同时测定花生中的黄曲霉毒素B1、B2、G1、G2

The aflatoxin B1, B2, G1, G2 in peanut were develop by LC-MS/MS. The mass spectrometer was operated in the positive ion mode using multiple reaction monitoring. The sample was extracted with methanol, and chromatographic separation was carried out on a MGIII-C₁₈ column(2.1 mm×150 mm×1.8 μm) with eluthic sion of V(acetonitrile):V(water)＝35:65. The limit of detection is 0.5 μg•L^－1, the limit of quantitation is 0.5 μg•kg^－1. The linear plots are between 0.5 μg•L^－1 and 25.0 μg•L^－1. Overall recoveries are between 88.3% and 99.2%, and RSD values are between 1.73％ and 3.75％.     

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.     

HPLC-MS/MS法同时检测牛奶中17种β2-受体激动剂和β-受体阻滞剂残留

A method for the determination of 17 β₂-agonists and β-blockers in milk was developed by solid-phase extraction(SPE) and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). The samples were extracted with acetontrile and cleaned with an Oasis MAX SPE cartridge, after protein precipitation with trichloracetate. The analytics were quantified by HPLC-ESI-MS/MS operating in positive multiple-reaction mode(MRM). Recoveries of 17 compounds range from 61.6 % to 134.3%, and the RSDs are less than 25%. LOD and LOQ of the analytics upon the method range from 0.024 to 3.960 μg kg^－1 and from 0.068 to 13.200 μg kg^－1.     

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%.     

超高效液相色谱-串联质谱法测定动物源性食品中性激素多组分残留

A rapid, specific and highly sensitive method for the simultaneous determination of seven sex hormones residueing in animal product was developed, which was based on UPLC-MS/MS under positive mode using electrospray ionization(ESI) source. ZnCl₂ was added to the extract solution to remove fat, and then target compounds were purified by LC-C₁₈ and LC-NH₂ solid phase extraction cartridge. Average recoveries for the seven sex hormone(spiked at the levels of 4 μg kg^－1 in fish product) range from 88% to 105%，with relative standard deviations between 4.3% and 24%.     

液相色谱与三重串联四极杆质谱联用技术用于动物源性食品中11种合成类固醇类激素的检测

A simple, rapid and specific analytical method for simultaneous determination of 11 kinds of steroid hormone including boldenone, methanodrosternolone, methyltestosterone, nandrolone, stanozolol, testosterone, trenbolone, nandrolone phenylpropionate, nandrolone propionat, progesterone, testosterone propionate was developed by Agilent 6410 LC-MS/MS. The LOD of target compounds is all lower than 0.1 μg kg^－1. The method is successfully applied to determination steroid hormone in chicken, shrimp and pork.     

电喷雾解吸电离质谱法直接测定纺织品中致癌性芳香胺

Using a mixture of V (methanol):V (water):V (acetic acid)＝49:49:2, as the electrospray liquid, under optimized experimental conditions, as 24 kinds of carcinogenic aromatic amines on various texture of textile samples were fast directly detected by DESI-MS non-destructive. During analyzing actual sample, the mean analysis time for a single sample is about 30 s due to the method without the sample pretreatment, so it can save a lot of analysis time and improve the efficiency of the analysis. At the same time, the DESI-MS/MS has the elimination of false positive alert in virtue of the DESI-MS/MS of differentia. The method has a high sensitivity for analyzing most aromatic amines, with typical values ranges in a few 10^－9 g•kg^－1.     

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.     

液相色谱-串联质谱法测定玉米中伏马菌素B1

Fumonisin B1 in maize was determined by liquid chromatography/tandem mass spectrometry. The analysis was extracted from maize samples by acetonitrile-water-acetic acid 49:50:1(V/V/V). Raw extracts were evaporated to dryness and dissolved with mobile phase, chromatographyed on a C₁₈ column, and detection was performed on a triple quadrupole tandem mass spectrometry with electrospray ionization source. The method has a limit of quantification of 10 µg•kg^－1 in maize samples. The calibration curve is linear in the range of 1-500 µg•L^－1. The mean recovery ranges from 94 % to 104 %, and the relative standard derivations are lower than 9%. The method is sensitive and specific to be applied for determination of fumonisin B1 in maize samples.