ABSTRACT
A method of ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry ( UPLC-Q-TOF MS) was developed to determine 35 kinds of illegally added chemical fungicides in pesticide formulations. The samples were pretreated based on the ultrasonic extraction by the solvent of methanol, and then separated on a Zorbax C18(100 mm×1. 8 mm, 2. 1 μm) column by a gradient elution with 0. 1% formic acid aqueous solution and acetonitrile as the mobile phase. The mass spectrometer was operated under positive mode. Under the optimal conditions, the recoveries at three spiked levels (0. 2, 0. 4, and 2. 0 mg/kg) were in the range of 81. 0%-101. 3% and the RSDs were 1. 0%-4. 4%. Based on the developed method, 100 samples were analyzed, and among which 6 samples were screened out chemical fungicides. The proposed method was high-efficient, accurate and reliable for the qualitatively screening of illegaly added chemical fungicides.
ABSTRACT
OBJECTIVE:To establish a rapid determination method for 9 kinds of glucocorticoid and 8 kinds of non-steroidal anti-inflammatory drugs illegally added into anti-rheumatic TCM patches. METHODS:UPLC-MS/MS method was adopted. The samples were separated on Acquity UPLC? BEN C18 column with methanol-water(90:10,V/V)as mobile phase at flow rate 0.4 mL/min. The column temperature was set at 30℃,and sample size was 1μL. The ionization mode was electrospray ion source(ESI):spray needle voltage of 5500 V,ion source spray GS1,GS2 pressure of 50,50 psi,ion source temperature of 500 ℃,scanning range of m/z 50-500. The multiple reaction monitoring(MRM)combined with information-dependent acquisition (IDA) and en-hanced product ion scanning(EPI)was used to rapid qualitative analysis. RESULTS:The detection limits for 17 kinds of chemical components were not more than 0.400 μg/mL. RSDs for precision,repeatability,stability tests were not more than 4.93%,7.69%, 9.57%,respectively. Diclofenac sodium was detected in the sample. CONCLUSIONS:The method is selective and sensitive. It is suitable for qualitative analysis of chemicals illegally added into anti-rheumatism TCM patches.
ABSTRACT
OBJECTIVE:To develop a method for simultaneous determination of 12 nonsteroidal anti-inflammatory drugs (NSAIDs) illegally added into antirheumatic TCM preparations.METHODS:UPLC-MS/MS was adopted.The determination was performed on Hypersil Golden C18 column with mobile phase consisted of 5 mmol/L ammonium formate solution-methanol (gradient elution) at the flow rate of 0.2 mL/min.The column temperature was 40 ℃,and the sample size was 2 μL.A tandem quadrupole mass spectrometer equipped with electrospray ionization source was used in positive-negative ion mode:curtain gas of 25 kPa,atomizing gas of 60 kPa,auxiliary gas of 55 kPa,electrospray voltage of 4 500 V,ion source temperature of 650 ℃.The multiple reaction monitoring mode was performed.RESULTS:The linear ranges of acetaminophen,acetylsalicylic acid,aminopyrine,meloxicam,ibuprofen,naproxen,lam acid,nimesulide,diclofenac,indomethacin,ketoprofen and celecoxib were 0.01-2.0 μg/ rnL (r=0.995 6),0.05-5.0 μg/mL (r=0.997 6),0.01-2.0 μg/mL (r =0.998 7),0.02-5.0 μg/mL (r=0.995 0),0.02-5.0 μg/mL (r =0.995 3),0.02-5.0 μg/mL(r=0.996 5),0.05-5.0 μg/mL(r=0.995 4),0.02-5.0 μg/mL(r=0.996 0),0.05-5.0 μg/mL(r=0.995 9),0.02-5.0 μg/mL(r=0.995 7),0.02-5.0 μg/mL(r=0.996 8),0.01-2.0 μg/mL(r=0.998 7),respectively.The limits of quantitation were no more than 0.20 mg/g,and the limits of detection were no more than 0.05 mg/g.RSDs of precision,stability and reproducibility tests were all lower than 5.0％.The recoveries were 80.8％-114.2％ (RSD was 3.85％-7.32％,n=9).CONCLUSIONS:The established method is simple,accurate,stable and reproducible,and can be used for simultaneous determination of 12 NSAIDs illegally added into antirheumatic TCM preparations.
ABSTRACT
OBJECTIVE:To develop a method for simultaneous determination of 12 nonsteroidal anti-inflammatory drugs (NSAIDs) illegally added into antirheumatic TCM preparations.METHODS:UPLC-MS/MS was adopted.The determination was performed on Hypersil Golden C18 column with mobile phase consisted of 5 mmol/L ammonium formate solution-methanol (gradient elution) at the flow rate of 0.2 mL/min.The column temperature was 40 ℃,and the sample size was 2 μL.A tandem quadrupole mass spectrometer equipped with electrospray ionization source was used in positive-negative ion mode:curtain gas of 25 kPa,atomizing gas of 60 kPa,auxiliary gas of 55 kPa,electrospray voltage of 4 500 V,ion source temperature of 650 ℃.The multiple reaction monitoring mode was performed.RESULTS:The linear ranges of acetaminophen,acetylsalicylic acid,aminopyrine,meloxicam,ibuprofen,naproxen,lam acid,nimesulide,diclofenac,indomethacin,ketoprofen and celecoxib were 0.01-2.0 μg/ rnL (r=0.995 6),0.05-5.0 μg/mL (r=0.997 6),0.01-2.0 μg/mL (r =0.998 7),0.02-5.0 μg/mL (r=0.995 0),0.02-5.0 μg/mL (r =0.995 3),0.02-5.0 μg/mL(r=0.996 5),0.05-5.0 μg/mL(r=0.995 4),0.02-5.0 μg/mL(r=0.996 0),0.05-5.0 μg/mL(r=0.995 9),0.02-5.0 μg/mL(r=0.995 7),0.02-5.0 μg/mL(r=0.996 8),0.01-2.0 μg/mL(r=0.998 7),respectively.The limits of quantitation were no more than 0.20 mg/g,and the limits of detection were no more than 0.05 mg/g.RSDs of precision,stability and reproducibility tests were all lower than 5.0％.The recoveries were 80.8％-114.2％ (RSD was 3.85％-7.32％,n=9).CONCLUSIONS:The established method is simple,accurate,stable and reproducible,and can be used for simultaneous determination of 12 NSAIDs illegally added into antirheumatic TCM preparations.
ABSTRACT
Objective:To establish a rapid, sensitive and accurate HPLC-QTOF/MS determination method for the illegally added antihypertensive drugs in traditional Chinese medicines and healthy care products .Methods:An Agilent Eclipse plus C 18 column ( 50 mm ×2.1 mm,1.8 μm) was adopted with the mobile phase of 0.5%formic acid and acetonitrile with gradient elution .The flow rate was 0.2 ml· min-1 .The electrospray ionization source was applied and operated in a positive ion mode .Results:The detection limit of 18 antihypertensive drugs was within the range of 0.2-2.5 ng· ml-1 .Reserpine was found in one sample .Conclusion:The method is selective and sensitive , which can be used for the detection of 18 chemical medicines illegally added in antihypertensive traditional Chinese medicines and health care products .
ABSTRACT
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.