Rapid identification 15 effective components of anti common cold medicine with MRM by LC-MS/MS / 药学学报

This paper reports the establishment of a method for rapid identification 15 effective components of anti common cold medicine (paracetamol, aminophenazone, pseudoephedrine hydrochloride, methylephedrine hydrochloride, caffeine, amantadine hydrochloride, phenazone, guaifenesin, chlorphenamine maleate, dextromethorphen hydrobromide, diphenhydramine hydrochloride, promethazine hydrochloride, propyphenazone, benorilate and diclofenac sodium) with MRM by LC-MS/MS. The samples were extracted by methanol and were separated from a Altantis T3 column within 15 min with a gradient of acetonitrile-ammonium acetate (containing 0.25% glacial acetic acid), a tandem quadrupole mass spectrometer equipped with electrospray ionization source (ESI) was used in positive ion mode, and multiple reaction monitoring (MRM) was performed for qualitative analysis of these compounds. The minimum detectable quantity were 0.33-2.5 microg x kg(-1) of the 15 compounds. The method is simple, accurate and with good reproducibility for rapid identification many components in the same chromatographic condition, and provides a reference for qualitative analysis illegally added chemicals in anti common cold medicine.

Content Determination of 5 Kinds of Amino Acids in Compound ?-Ketoacid Tablets by HPLC after Pre-column Programming Derivatization / 中国药房

OBJECTIVE: To establish an HPLC method with pre-column programming derivatization for the content determination of 5 kinds of amino acids in Compound ?-ketoacid tablets.METHODS: The separation was performed on C8 column(gradient elution) with column temperature at 40 ℃.OPA was used as the derivation reagent.The detection wavelength was set at 338 nm.The contents of L-lysine acetate,L-threoine,L-tryptophan,L-histidine,L-tyrosine in Compound ?-ketoacid tablets were determined.RESULTS: The linear ranges of L-lysine acetate,L-threoine,L-tryptophan,L-histidine,L-tyrosine were 0.10～5.25 mg?mL-1(r=0.999 9),0.052～2.65 mg?mL-1(r=0.999 8),0.022～1.15 mg?mL-1(r=0.999 9),0.038～1.91 mg?mL-1(r=0.999 7),0.030～1.51 mg?mL-1(r=1.000 0),respectively.The average recovery was 99.8%～100.1%(RSD=0.1%).CONCLUSION: This method is exclusive,sensitive and reliable for the content determination of amino acids in Compound ?-ketoacid tablets.

Improvement of Content Determination of Rocuronium Bromide by Potentiometric Titration / 中国药房

OBJECTIVE:To establish a mercury-free perchloric acid potentiometric titration method for the content determination of rocuronium bromide.METHODS:Mettler DG113-SC was used as the composite electrode.The potentiometric titration was performed with glacial acetic acid and acetic anhydride as solvents and perchloric acid(0.1 mol?L-1) as titration.The method was compared with that stated in European Pharmacopeia.RESULTS:The linear range of rocuronium bromide was 0.150 1～0.401 3 g(r=0.999 9) with an average recovery within 99.90%～99.98%.The detection limit was 1.71 mg.There was no difference between results detected by two methods.CONCLUSION:The method is simple,sensitive and accurate for the content determination of rocuronium bromide.

Determination of Residual Organic Solvents in Meropenem by Headspace Gas Chromatography / 中国药房

OBJECTIVE:To develop a headspace GC method for determination of residual organic solvents invovling methanol,alcohol,acetone,acetonitrile,dichloromethane and n-butanol in meropenem.METHODS:The residual organic solvents were separated on DB-624 capillary column using temperature programming.FID was used as detector with a temperature of 250 ℃ with nitrogen as carrier gas and water as solvent.The inlet temperature was 200 ℃.RESULTS:The linear range were 12～600 ?g?mL-1 (r=0.999 8) for methanol,20～1 000 ?g?mL-1 (r=0.999 9) for alcohol,20～1 000 ?g?mL-1 (r=0.999 9) for acetone,1.64～82 ?g?mL-1 (r=0.999 8) for acetonitrile,2.4～120 ?g?mL-1 (r=0.999 6) for dichloromethane and 20～1 000 ?g?mL-1 (r=0.999 9) for n-butanol with RSD of 1.0%,2.2%,0.9%,2.2%,1.6%,1.1%,respectively.The average recoveries were ranged from 98.8% to 99.6%.The LOD were about 0.06～0.43 ng.The residual levels of six organic solvents in 3 batches samples were all up to the standard stated in Chinese Pharmacopeia (2005 edition).CONCLUSION:The method is simple,accurate,sensitive and reproducible for determination of residual organic solvents in meropenem.

Determination of the Content of Glucose in Glucose/Sodium Chloride Injection by HPLC / 中国药房

OBJECTIVE:To establish an HPLC method for the determination of the content of glucose in Glucose/Sodium Chloride injection.METHODS:The determination was performed on Waters Sugar PakⅠ column with column temperature set at 80 ℃,water as mobile phase and injection volume of 20 ?L.The cell temperature of RID detector was set at 40 ℃.RESULTS:The linear range of glucose was 0.05～2.50 mg?mL-1(r=0.999 9) with the lowest detection limit of 24 ng.The average recovery ranged from 99.80% to 99.90%(RSD=0.21%).CONCLUSION:The method is simple,rapid,accurate,sensitive and reliable in operation,and it is applicable for determination of glucose in Glucose/Sodium Chloride injection.