• Archives of Pharmacal Research
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• v.17 no.6
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• pp.415-419
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• 1994

A simple nad rapid colorimetric method for the assay of amodiaquine hydrochloride, chloroquine phosphate and primaquine phosphate is described. The method is based on the interaction of the drug base with bromophenol blue to give a ion-pair complex. The spectra of the complex shows a maxima at 415-420 nm with high apparent molar absorptivities. Beer's law was obeyed in the concentration range 1-8, 2-10 and $2-12{\;}{\mu}{\cdot}ml^{-1}$ for amodiaquine hydrochloride, primaquine phosphate and chloroquine phosphate respectively. The proposed method was applied to the determination of these drugs in certain formulations and the results were favourably comparable to the official methods.

• Analytical Science and Technology
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• v.30 no.1
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• pp.39-48
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• 2017

Roxithromycin (RXT), which is an antibiotic used to treat respiratory tract and urinary infections, is official in Korean Pharmacopoeia (KP) and is marketed in various dosage forms including tablet, granule, suspension, and tablet for suspension in Korea. This study presents how a universal and reliable method to quantify RXT in bulk drug and formulations was developed. Effects of factors including column type, buffer concentration, type and concentration of organic solvent, buffer pH, and type and concentration of mobile phase additive, were examined, and some categorical or crucial factors including the types of column, organic solvent, mobile phase additive and the buffer pH were optimized by one-factor-at-a-time approach. Subsequently, concentrations of the buffer and additive and column temperature were optimized by response surface methodology using Box-Behnken design aiming to acquire the RXT peak of good shape. The optimized method employed a Phenomenex Gemini $5{\mu}$ C18 110A ($150{\times}4.60mm$, $5{\mu}m$) maintained at $30^{\circ}C$ with the mobile phase consisting of 25 mM phosphate buffer (pH 6.0) with 0.3 % tetrabutylammonium hydroxide and methanol at a ratio of 37:63 (v/v). Method validation results showed that the developed method was linear, precise, and accurate. Compared to the compendial methods in KP 10 that exhibited a significant tailing of the RXT peak despite using unfavorably high buffer concentrations and were not harmonized among bulk drug and formulations, this method could be universally applied to RXT bulk drug and marketed products in various dosage forms and thus was adopted in KP 11.

• Analytical Science and Technology
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• v.13 no.5
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• pp.675-682
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• 2000

The concentration of dioxins from flue gases of municipal waste incineration facilities with capacities over 50 tons/day are regulated by the guideline: $0.1ng-TEQ/Nm^3$ for new facilities, and $0.5ng-TEQ/Nm^3$ for existing facilities and it will be strengthened to $0.1ng-TEQ/Nm^3$ until 2003 year. Dioxins from these incineration facilities have to be measured more than 2 times annually by the Official Test Facilities of Dioxins. Seven institutions have been certified so far as the Official Test Facilities of Dioxins. These facilities have to be evaluated by the quality control program provided by National Institute of Environmental Research every year. We reported the results of quality control test performed in 1999. Four institutions certified in 1998 sampled flue gases at stack of M incineration facilitiy and analyzed dioxins by Official Methods of Air Pollution. The isokinetic coefficients, the parameter for evaluation of sampling ability were excellent for all four institutions. They were 100.9%, 102.4%, 102.1% and 99.2%, respectively. The criteria required are as follows; resolution over 10,000, mass calibration within ${\pm}5ppm$, ion abundance ratio within 15%, and the recovery of 50-120%. As results, those institutions also met these parameters of Official Method of Air Pollution.

• Journal of Food Hygiene and Safety
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• v.30 no.3
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• pp.272-280
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• 2015

A simultaneous official method was developed for the determination of phorate and its metabolites (phorate sulfoxide, phorate sulfone, phorate oxon, phorate oxon sulfoxide, phorate oxon sulfone) in livestock samples. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Phorate and its metabolites were extracted from beef and milk samples with acidified acetonitrile (containing 1% acetic acid) and partitioned with anhydrous magnesium sulfate. Then, the extract was purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/L) for all the analytes into blank extract with $r^2$ > 0.996. For validation purposes, recovery studies were carried out at three different concentration levels (beef 0.004, 0.04 and 0.2 mg/kg; milk 0.008, 0.04 and 0.2 mg/kg, n = 5). The recoveries were within 79.2-113.9% with relative standard deviations (RSDs) less than 19.2% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines. The limit of quantification was quite lower than the maximum residue limit (MRL) set by the Ministry of Food and Drug Safety (0.05 mg/kg). The proposed analytical method was accurate, effective and sensitive for phorate and its metabolites determination and it will be used to as an official analytical method in Korea.

• Analytical Science and Technology
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• v.30 no.1
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• pp.32-38
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• 2017

In attempt to contribute in official monographs of Korean Pharmacopoeia, an HPLC method was developed and fully validated for the determination of tolperisone hydrochloride in tablets which have never been published in other forgein Pharmacopoeia. Analysis was carried out in an ODS column ($250{\times}4.6mm$ I.D., $5{\mu}m$) with common solvents include acetonitrile and ammonium hydrophosphate buffer as mobile phase. The assay was validated according to International Conference on Harmonization (ICH) guidelines. The method has good linearity in the range of $5-200{\mu}g/mL$ tolperisone. Intra-day precision varied between 0.04 and 0.10 %. Relative standard deviations of inter-day precision ranged between 0.43 and 1.24 % for peak area. The percentage recovery of the tolperisone ranged between 99.8 and 101.2 % in material. Recoveries in tablets were ranged between 98.7 and 100.8 %, thus confirmed the suitability of method for estimation of tolperisone hydrochloride in tablet dosage form.

• Analytical Science and Technology
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• v.14 no.2
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• pp.173-179
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• 2001

The study was carried out to analyze the pollutant Fe, Cu, Cr, Zn, Cd for sediments collected from lake in K river basin. Three analytical methods currently used in Korea, Japan, U.S.A, were compared. Pretreatment using microwave digestion showed higher analytical results for Fe, Cu, Cr, Zn, Cd than Korean Official Method(KOM) and American Toxicity Characteristic Leaching Procedure(TCLP) Method. Also, analytical results using microwave digestion, TCLP and KOM were as follows: 38.1-48.0 mgFe/kg, 10.2-15.9 mgFe/kg AND 3.5-12.6 mgFe/kg, 37.0-50.1 mgCu/kg, 0.06-0.24 mgCu/kg and 0.01-0.03 mgCu/kg, 137.0-152.0 mgZn/kg, 0.67-0.82 mgZn/kg and 0.3-0.5 mgZn/kg, respectively. From this result, a new analytical method for the determination of heavy metal in sediment should be developed for the accurate estimation of pollution degree in sediment.

• Analytical Science and Technology
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• v.33 no.6
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• pp.252-261
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• 2020

Currently, the potentiometric titration and the high pressure liquid chromatography (HPLC) method were utilized in Korean Pharmacopoeia XII (KP XII) as well as other pharmacopoeias (USP, EP, BP) for determination of loperamide hydrochloride in raw materials and capsules, respectively. The research objective is to overcome the remaining drawbacks from current methods such as solubility of mobile phase (KP XII), less scientific approach (USP 43) or using paired-ion chromatography reagent which shows some limitations (BP2017 and other formulation monographs). The proposed method was optimized by Design of Experiment (DoE) tool to obtain the satisfied method for determination of loperamide hydrochloride. The optimal condition was performed on the common C18 column (150 mm × 4.6 mm; 5 ㎛) using isocratic elution with the mobile phase containing 40 mM of potassium phosphate monobasic (pH 3.0) and acetonitrile (56:44), at a flow rate of 0.7 mL/min. The optimized method was validated and met the requirements of the International Conference on Harmonization. The developed method was applied to determine loperamide hydrochloride in capsules and can be used to update the current monograph in KP XII.

• Analytical Science and Technology
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• v.30 no.3
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• pp.154-158
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• 2017

The Korean Pharmacopoeia (KP XI), British Pharmacopoeia (BP 2013) and Japanese Pharmacopoeia contain monographs for the quality control of raw fusidate sodium and its formulations using high performance liquid chromatography (HPLC). However, the assay method for the determination of fusidate sodium in commercial tablets is titration which is less specific than HPLC. In this study, we present an alternative HPLC method for quantitation of fusidate sodium in tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9999$), while the RSDs for intra- and inter-day precision were 0.25-0.37 % and 0.11-0.60 %, respectively. Accuracies ranged from 99.46-100.85 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

• Analytical Science and Technology
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• v.30 no.5
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• pp.221-225
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• 2017

Thioctic acid is a vitamin-like antioxidant which is prepared as tablets and injection. The Korean Pharmacopoeia (KP XI) contains monograph for the quality control of raw thioctic acid using ultra-violet visible spectrophotometry and its formulations using high performance liquid chromatography (HPLC). In British Pharmacopoeia 2013 (BP2013), another HPLC method is used for the assay test of thioctic acid material. For the international harmonization, we present an HPLC method for quantitation of thioctic acid in both raw material and tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9995$), while the RSDs for intra- and inter-day precision were 0.93 ~ 1.26 % and 1.40 ~ 1.76 %, respectively. Accuracies ranged from 98.13-100.00 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

• The Korean Journal of Pesticide Science
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• v.17 no.2
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• pp.107-116
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• 2013

Polar pesticides like pymetrozine (log $P_{ow}$: -0.18) are known to be difficult to analyze. The analytical method of pymetrozine using hydromatrix included in the official method of KFDA was uncommon and provided ambiguous evidence to confirm both the identity and the quantity. Therefore, precise single residue analytical method was developed in representative crops for using liquid-liquid extraction (LLE). The pymetrozine residue was extracted with methanol from 11 representative crops which comprised apple, blueberry, broccoli, cabbage, cherry, crown daisy, hulled rice, Korean cabbage, potato, rice and watermelon. The extract was purified serially by liquid-liquid extraction (LLE) and silica solid phase extraction (SPE). For rice and hulled rice samples, n-hexane partition was additionally adopted to remove nonpolar interferences, mainly lipids. The residue levels were analyzed by HPLC with DAD, using $C_8$ column. LOQ (limit of quantitation) of pymetroizinie was 1 ng (S/N > 10) and MQL (method quantitation limit) was 0.01 mg/kg. Mean recoveries from 11 crop samples fortified at three levels (MQL, 10 ${\times}$ MQL and 50 ${\times}$ MQL) in triplicate were in the range of 83.1~98.5% with coefficients of variation (CV) of less than 10%, regardless of sample type, which satisfies the criteria of KFDA. The method established in this study could be applied to most of crops as an official and general method for analysis of pymetrozine residue.