Simultaneous detection of hazardous skin whitening agents in Indian cosmetic products using a green chromatographic technique

The present work mainly highlights the simultaneous detection of four skin whitening agents i.e. hydroquinone (HQ), resorcinol (RS), catechol (CC) and 3,3′-dichlorobenzidine (DCB) in facial creams and body lotion. Among these, the first three are positional isomers of dihydroxybenzene so simultaneous separation is difficult with the conventional reverse-phase high-performance liquid chromatographic technique (RP-HPLC). The selected skin whitening agents were detected in facial cream and body lotion using micellar liquid chromatography coupled to a photodiode array detector (MLC-PDA). In the present study, optimization of the method was accomplished using response surface methodology (RSM) with central composite design (CCD). The second-order polynomial model for predicting the optimal chromatographic run time was evaluated by the analysis of variance (ANOVA) and 3D response surface plots for the interactions between three variables were constructed. Three experimental parameters which were chosen as independent variables were; surfactant concentration (SDS), the volume percentage of organic modifier (OM) and pH of the mobile phase. The second-order polynomial model for predicting the optimal chromatographic run time was evaluated by the analysis of variance (ANOVA) and 3D response surface plots for the interactions between three variables were constructed. Three experimental parameters which were chosen as independent variables were; surfactant concentration (SDS), percentage of organic modifier (OM) and pH of the mobile phase. The second-order polynomial model for predicting the optimal chromatographic run time was evaluated by the analysis of variance (ANOVA) and 3D response surface plots for the interactions between three variables were constructed. Three experimental parameters which were chosen as independent variables were; surfactant concentration (SDS), percentage of organic modifier (OM) and pH of the mobile phase. The optimized mobile phase was 0.15 M SDS and 7% 1-butanol, buffered at pH 7 with 0.01 M NaH2PO4. The chromatographic run time for simultaneous determination of selected analytes was 7.5 min. The correlation coefficient (r2) values were satisfactory between 0.998–0.999 over the linear concentration range. Limits of detection (LODs) and the limits of quantification (LOQs) for the four skin whitening agents were in the range of 0.05–0.07 μg/mg and 0.11–0.14 μg/mg, respectively. Trueness (98.4–102.7%) and precision (< 4.3%) were acceptable. The developed method was fast, cost-effective, and green which could easily analyze complex matrices (facial creams, body lotion) without any pretreatment other than filtration. The results indicated that the MLC-PDA method proved to be more suitable for the simultaneous separation of selected positional isomers

Detection of most commonly used pesticides in green leafy vegetables from sagar, india using direct injection hybrid micellar liquid chromatography

Imidacloprid, chlorpyrifos, profenofos and cypermethrin are most commonly applied pesticides on green leafy vegetables. After a survey conducted to know the pesticide management practices in Sagar, India, a procedure based on hybrid micellar liquid chromatography coupled to a photodiode array detector has been developed and validated to monitor imidacloprid, chlorpyrifos, profenofos and cypermethrin content in green leafy vegetables. The method was validated following the guideline of SANTE/11,312/2021 in terms of: selectivity, linearity (r2> 0.998), limit of quantification (0.09–0.25 mg/Kg, depending on the analyte under investigation), precision (<8.1%), and robustness (<5%). Chlorpyrifos was found to be the most commonly used pesticide among vegetable growers. It was found in seventy-six percent samples, profenofos in fifty-one percent, imidacloprid in eight percent and cypermethrin in four percent of the analyzed green leafy vegetable sample either individually or in combination. Sixteen percent of the collected samples were found to be negative for the selected pesticides. The developed procedure is rapid, easy to handle, green since it uses a low amount of toxic chemicals providing reliable results. The method was used to evaluate the eventual correlation between the analytical data and the information collected from the producers and users of these pesticides.The authors are thankful to DST-FIST and DST-PURSE (Department of Science and Technology; Government of India) for supporting with FIST and PURSE scheme (Sl.No.64 Dated 31–05–2016). Work supported by Grant PID2019-106708GB-I00 funded by MCIN (Ministry of Science and Innovation of Spain)/AEI/10.13039/501100011033. Hemlata Bhamdare [UGC-Ref.No.3354/(OBC)(NET-DEC.2015)] and Priyanka Pahade [UGC-Ref.No.3335/(Sc) (NET-DEC.2015)] are grateful to University Grant Commission (UGC) for providing a Senior Research Fellowship

A survey based on the use of imidacloprid on green leafy vegetables in remotely located Sagar, India

The low literacy level of the vegetable growers in the selected region of India is responsible for the use of highly toxic organophosphate pesticides on green leafy vegetables. Although in the Indian market imidacloprid (less toxic) is available but due to its high price and less effectiveness compared to that of organophosphates is not preferred to control pests on green leafy vegetables. The present research is a survey-based study designed to know the insecticide management practice among insecticide dealers, vegetable growers and comparison of obtained information with chromatographic results. The combination of survey and instrumental method (micellar liquid chromatographic technique) was utilized to determine whether the information collected from vegetable growers and insecticide dealers were similar and signicantly correlated with analytical data or not. Among the selected 48 samples of green leafy vegetables, imidacloprid was detected only in 6 samples. The survey of the insecticide dealers and vegetable growers conrmed that the vegetable growers used toxic organophosphates pesticides instead of less toxic imidacloprid. Survey data collected from vegetable growers and pesticide dealers were also tested by chromatographic method and a signicant correlation was found between them, which clearly demonstrates the minimum use of safe insecticide (imidacloprid). Imidacloprid insecticide was detected on green leafy vegetables after a preliminary survey of vegetable growers and pesticide dealers. Survey results revealed the use of potentially harmful pesticides other than imidacloprid which are banned from using in vegetables. Analytical results showed signicantly less use of imidacloprid on green leafy vegetables

Screening of some banned aromatic amines in textile products from Indian bandhani and gamthi fabric and in human sweat using micellar liquid chromatography

Certain dyes in textile products, which are capable of reductively splitting into carcinogenic aromatic amines, are strictly controlled in many countries. A simple, rapid, sensitive and green chromatographic method has been developed and validated for the simultaneous determination of 4-aminophenol (4-AMP), p-phenylenediamine (p-PPD) and benzidine (BNZ), banned aromatic amines in dyeing clothes and human sweat. The separation was achieved using a micellar mobile phase of 0.1 M SDS, 4% 1- butanol (v/v) buffered to pH 7 with sodium dihydrogen phosphate, flowing under isocratic mode at 1 mL/min through a C18 column. Photodiode array detector was set at 210 nm. Using the above chromatographic conditions, 4-AMP, p-PPD and BNZ were eluted at 3.5 min, 4.7 min. and 5.4 min., respectively, adequately resolved. The method was validated by Standard Practices for Method Validation in Forensic Toxicology guideline for the industry in terms of selectivity, calibration curve, linearity (r2 = 0.999), trueness (relative bias, −3.5 to 7%) precision (relative standard deviation, <8.5%), and robustness of selected compounds. This method was sensitive enough for the routine analysis of aromatic amine in textile material with limit of detection in the (0.01 to 0.04 μg/mL range and limit of quantification (0.03-0.13 μg/mL). The method was successfully applied to dyed clothes and sweat samples. The main advantage of the developed method is the easy extraction step of the analytes from incurred samples without any further cleanup, which reduces per sample analysis cost and the total time of analysis. The developed method could easily replace regular chromatographic technique used for their detection

Application of micellar liquid chromatographic method for rapid screening of ceftriaxone, metronidazole, amoxicillin, amikacin and ciprofloxacin in hospital wastewater from Sagar District, India

The present research work mainly highlights the simultaneous detection of five antibiotics i.e., ceftriaxone (CTX), metronidazole (MTZ), amoxicillin (AMX), amikacin (AMK) and ciprofloxacin (CPFX) in hospital wastewater located in Sagar district (Madhya Pradesh, India). All these antibiotics make their way through drainage systems into the environment in the form of metabolized and unmetabolized compounds. Growing concern about the antibiotic resistance and contamination of wastewater by antibiotics requires fast, sensitive and eco‐friendly techniques. Therefore a simple, rapid and eco‐friendly chromatographic method has been developed for simultaneous determination of CTX, MTZ, AMX, AMK and CPFX in hospital wastewater samples. Optimization of the method was accomplished using response surface methodology (RSM) with Box‐Behnken design (BBD). The optimized mobile phase was 0.15 M SDS‐0.01 M NaH2PO4‐7% (v/v) 1‐butanol, pH 3 which provided a chromatographic run time of 11 min. for the simultaneous determination of selected antibiotics. The correlation coefficient (r2 ) values were satisfactory between 0.996 and 0.999 over the linear concentration range of 0.04–12 μg/mL. Limits of detection (LODs) and the limits of quantification (LOQs) for the five antibiotics were in the range of 0.02–0.18 μg/ mL and 0.04–0.25 μg/mL, respectively. The developed method is simple, rapid, cost‐effective and green which could be used for complex matrix (wastewater) without any sample pretreatment other than filtration. The results indicated that the MLC‐PDA method proved to be more suitable than reverse phase‐high performance liquid chromatography for the simultaneous separation of selected antibiotics

Micellar enhanced chromatographic separation of selected hazardous chemical present in hair dye and their detection in formulations and swab, including assessment of damage caused to cuticle of hair shaft

Hydroquinone (HQ), resorcinol (RS), m-aminophenol (m-AMP) and p-phenylenediamine (p-PPD) are aromatic compounds which are generally used in hair dyes to provide different colours to hair. In European Union the concentrations of HQ, RS, m-AMP and p-PPD is regulated in hair dyes and other cosmetic products by EU commission regulation EU/2019/831. This legislation is generally exercised because all these compounds are toxic and may cause severe allergies when used regularly. However in India no such regulations exist to monitor these toxic compounds in hair dyes therefore in this study a simple, rapid, economical and ecofriendly micellar liquid chromatographic (MLC) technique has been developed which can monitor all the selected toxic compounds simultaneously. HQ and RS are positional isomers and are difficult to be separated by HPLC whereas with the developed MLC method it was well separated and detected. The developed MLC technique has been applied to detect and quantify selected analytes in oxidative and non-oxidative hair dyes and swab samples from the scalp. The simultaneous separation of selected analytes was performed in mobile phase 0.09 M SDS, 0.01 M NaH2PO4–2% v/v 1-butanol at pH 7 running through C18 column under isocratic mode at 1 mL/min. flow rate. All the analytes were eluted within 6 min. The present method has been validated following the EURCHEM Guideline, 2014 in terms of calibration range (0.08–15 µg/mL), limit of detection (0.01–0.09 µg/mL), limit of quantification (0.08–0.35 µg/mL), accuracy (<5.6%), precision (91–105%) and robustness (<5.8%). The selected compounds in hair dye formulation were found in the range of 0.06–12.2 µg/mL (when diluted 25 times). Hair dyes persistence study was conducted up to 10 days from the day of application on the scalp, suggesting that the dyes were not completely washed off and were retained on the scalp for more than one week. SEM analysis of dyed hair revealed that hair are severely damaged due to use of dyes. The advantage of the developed method is that it could easily be adopted by quality control and cosmetic laboratories for quality control and check for the simultaneous separation of positional isomers together with two other aromatic compounds

Direct injection green chromatographic method for simultaneous quantification of amoxicillin and amikacin in maternity hospital wastewater (Sagar, India)

Amoxicillin (AMO) and amikacin (AMK) are broad-spectrum antibiotics that are most preferably given post-delivery (normal and cesarian) in the maternity hospitals located in Sagar city (Madhya Pradesh), India. Both the antibiotics make their way through sewage/drainage systems into the environment in the form of metabolized and unmetabolized compounds. Growing concern about the contamination of wastewater by antibiotics requires fast, sensitive and eco-friendly techniques. Therefore a simple, rapid and environmental friendly chromatographic method has been developed for simultaneous determination of AMO and AMK in maternity hospital wastewater samples. A micellar liquid chromatographic (MLC) method was developed with a C18 column (250 mm × 4.6 mm), sodium dodecyl sulphate (SDS; 0.15 M), 1-butanol (7%) as a modifier, pH 5 and photo diode detector (PDA) at 270 nm and 256 nm for AMO and AMK respectively. The method was fast with analysis time below 9 min. In the present MLC method, linearities (r > 0.998), limits of quantification in the range of 0.02–0.04 μg/mL, repeatabilities, and intermediate precision below 4.9% were adequate for the quantification of AMO and AMK. The proposed method can be utilized to detect and quantify both the antibiotics in various samples by hospitals, pharmaceutical companies, pollution control board, municipal corporations, etc

Screening of some banned aromatic amines in textile products from Indian bandhani and gamthi fabric and in human sweat using micellar liquid chromatography

Certain dyes in textile products, which are capable of reductively splitting into carcinogenic aromatic amines, are strictly controlled in many countries. A simple, rapid, sensitive and green chromatographic method has been developed and validated for the simultaneous determination of 4-aminophenol (4-AMP), p-phenylenediamine (p-PPD) and benzidine (BNZ), banned aromatic amines in dyeing clothes and human sweat. The separation was achieved using a micellar mobile phase of 0.1 M SDS, 4% 1- butanol (v/v) buffered to pH 7 with sodium dihydrogen phosphate, flowing under isocratic mode at 1 mL/min through a C18 column. Photodiode array detector was set at 210 nm. Using the above chromatographic conditions, 4-AMP, p-PPD and BNZ were eluted at 3.5 min, 4.7 min. and 5.4 min., respectively, adequately resolved. The method was validated by Standard Practices for Method Validation in Forensic Toxicology guideline for the industry in terms of selectivity, calibration curve, linearity (r2 = 0.999), trueness (relative bias, −3.5 to 7%) precision (relative standard deviation, <8.5%), and robustness of selected compounds. This method was sensitive enough for the routine analysis of aromatic amine in textile material with limit of detection in the (0.01 to 0.04 μg/mL range and limit of quantification (0.03–0.13 μg/mL). The method was successfully applied to dyed clothes and sweat samples. The main advantage of the developed method is the easy extraction step of the analytes from incurred samples without any further cleanup, which reduces per sample analysis cost and the total time of analysis. The developed method could easily replace regular chromatographic technique used for their detection