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Huang Y.-Y.,Jiaxing University | Tu J.-H.,Jiaxing University | Xu H.-X.,Jiaxing Institute for Food and Drug Control | Fu Y.-H.,Jiaxing University
Chinese Traditional and Herbal Drugs | Year: 2016

Objective: To estabilsh a rapid and accurate method for the determination of 17 anti-inflammatory and analgesic chemicals (paracetamol, aspirin, phenacetin, chlorpheniramine maleate, rofecoxib, piroxicam, lornoxicam, meloxicam, prednisone acetate, sulindac, naproxen, dexamethasone acetate, phenylbutazone, oxaprozin, celecoxib, diclofenac sodium, and indomethacin) which were illegally added into the Chinese patent medicines (CPM) and the health foods. Methods: The UPLC-MS/MS method was adopted. The samples were extracted with methanol by ultrasonic processing and separated on a Waters Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with 0.1% formic acid methanol (A) and 0.1% formic acid water (B) as the mobile phase by gradient elution (0-4 min, 40% A; 4-5 min, 40%-50% A; 5-6 min, 50%-60% A; 6-12 min, 60%-80% A; 12-13 min, 80% A; 13-14 min, 80%-40% A) at a flow rate of 0.2 mL/min, and the column temperature was 40℃. A positive-ion (ESI+) source and a MRM mode were used to separately and quantitatively determinate the 17 anti-inflammation and analgesia chemicals. The obtained molecular ions, fragment ions, and retention time for MRM channels were used to identify the 17 chemicals by comparison with those of reference substances. The obtained peak areas were used to determinate the accurate content of chemicals in commonly used drugs in clinic. Results: A good resolution of the 17 chemicals, including paracetamol, aspirin, phenacetin, chlorpheniramine maleate, rofecoxib, piroxicam, lornoxicam, meloxicam, prednisone acetate, sulindac, naproxen, dexamethasone acetate, phenylbutazone, oxaprozin, celecoxib, diclofenac sodium, and indomethacin was obtained under this UPLC and MS/MS condition. The limits of qualitation and quantitation were in the range of 0.3-5.0 and 0.9-15.0 ng/g. The standard addition recoveries were in the range of 90.5%-113.8%. The six components in samples (paracetamol, prednisone acetate, diclofenac sodium, indometacin, chlorpheniramine maleate, and naproxen) were detected. Conclusion: The method is simple, accurate, and has high sensitivity, which can be used for the qualitative and quantitative determination of illegally added chemicals in CPM and health foods. © 2016, Editorial Office of Chinese Traditional and Herbal Drugs. All right reserved.


Jiang L.-P.,Jiaxing Institute for Food and Drug Control | Tu J.-H.,Jiaxing University | Xu H.-X.,Jiaxing Institute for Food and Drug Control | Fu Y.-H.,Jiaxing University
Chinese Traditional and Herbal Drugs | Year: 2015

Objective: To establish an accurate method for the determination of nine chemical drugs (phentolamine mesylate, methyltestosterone, stanozolol, danazol, tadalafil, sildenafil citrate, aildenafil, vardenafil, and thioaildenafil) which were illegally added into the antifatigue health foods. Methods: The UPLC-MS/MS method was adopted. The samples were extracted with methanol by ultrasonic processing and separated on a Waters Acquity BEH-C18 (100 mm × 2.1 mm, 1.7 μm) column with 0.1% formic acid methanol (A) and 0.1% formic acid water (B) as the mobile phase by gradient elution (0-5 min, 50% A; 5-7 min, 50%-90% A; 7-9 min, 90%-100% A; 9-10 min, 100%-50% A) at a flow rate of 0.2 mL/min. The injection volume was 5 μL. The column temperature was 40 ℃. The positive-ion (ESI+) source and MRM mode were used to separate and quantitatively determine the chemicals. The obtained molecular ions, fragment ions, and retention time for MRM channels were used to identify the nine kinds of drugs by comparing with those of reference substances. The obtained peak areas were used to determine the accurate content of the nine chemicals in the antifatigue health foods. Results: A good resolution of the nine kinds of chemical drugs, including phentolamine mesylate, methyltestosterone, stanozolol, danazol, tadalafil, sildenafil citrate, aildenafil, vardenafil, and thioaildenafil, was obtained under this UPLC and MS/MS conditions. The limits of detection (LOD) and quantification (LOQ) were in the ranges of 0.1-0.3 ng/g and 0.3-0.9 ng/g. The standard addition recoveries were in the range of 88.4%-116.3%. There were 68 batches of antifatigue health foods, among which 41 batches were added with the chemicals with positive rate of 60.3%. The sildenafil citrate, tadalafil, aildenafil, and hioaildenafil were detected in samples. Conclusion: The method is simple, accurate, and has high sensitivity, which can be used for the qualitative and quantitative determination of illegally added chemical drugs in the antifatigue health foods. © 2015, Editorial Office of Chinese Traditional and Herbal Drugs. All right reserved.


Ding B.-Y.,Jiaxing University | Tu J.-H.,Jiaxing University | Xue L.-B.,Jiaxing Institute for Food and Drug Control | Xu H.-X.,Jiaxing Institute for Food and Drug Control | Fu Y.-H.,Jiaxing University
Chinese Traditional and Herbal Drugs | Year: 2015

To establish a rapid and accurate method for the determination of 34 chemical hypotensors which were illegally added into the blood pressure lowering class Chinese patent medicines (CPM) and the blood pressure regulating class health foods. The UPLC-MS/MS method was adopted. The samples were extracted with methanol by ultrasonic processing and separated on a Waters Acquity BEH-C18 (100 mm × 2.1 mm, 1.7 μm) column with 0.1% formic acid methanol (A) and 0.1% formic acid water solution (B) as the mobile phase by gradient elution (0-5 min, 32% A; 5-8 min, 32%-50% A; 8-12 min, 50% A; 12-14 min, 50%-60% A; 14-16 min, 60%-80% A; 16-18 min, 80% A; 18-19 min, 80%-90% A; 19-20 min, 90%-100% A; 20-21 min, 100% A; and 21-22 min, 100%-32% A) at a flow rate of 0.2 mL/min, and the column temperature was 40℃. A positive-ion (ESI+) source and a MRM mode were used to separate and quantitatively determine the chemical hypotensors. The obtained molecular ions, fragment ions, and retention time for MRM channels were used to identify the 34 kinds of drugs by comparison with those of reference substances. The obtained peak areas were used to determine the accurate content of chemical hypotensors in the blood pressure lowering class CPM and the blood pressure regulating class health foods. A good resolution of 34 kinds of chemical drugs, including clonidine, captopril, yohimban-16-carboxylicacid, L-tyrosine, hydrochlorothiazide, furosemide, indapamide, minoxidil, hydralazine, atenolol, lisinopril, dibazole, metoprolol, bisoprolol, prazosin, terazosin, propranolol, enalapril, quinapril, benazepril, dilthiazem, doxazosin, nicardipine, nifedipine, amlodipine, nimodipine, felodipine, nitrendipine nisoldipine, valsartan, telmisartan, candesartan cilexetil, rbesartan, and olmesartan medoxomil was obtained under this UPLC and MS/MS condition. The limits of qualitative and quantitative were in the range of 0.1-0.5 and 0.3-1.5 ng/g. The standard addition recoveries were in the range of 81.4%-118.9%. The method is simple, accurate, and with high sensitivity, which can be used for the determination of illegally added chemical hypotensors in CPM and health foods. ©, 2015, Chinese Traditional and Herbal Drugs. All right reserved.

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