Highly Sensitive Detection of Pharmaceuticals and Personal Care Products (PPCPs) in Water Using Agilent 6495 Triple Quadrupole Mass Spectrometer
Oral Presentation
Prepared by C. Marvin1, M. Murphy2, D. Yang3
1 - Agilent Technologies, Inc., 2850 Centerville Road, Wilmington, DE, 19808, United States
2 - EPA Region 8 lab, 16194 West 45th Drive, Golden, CO, 80403, United States
3 - Agilent Technologies, Inc., 5301 Stevens Creek Blvd, Santa Clara, CA, 95051, United States
Contact Information: [email protected]; 408-553-7091
ABSTRACT
PPCPs comprise a diverse collection of thousands of chemical substances, including prescription and over-the-counter therapeutic drugs, veterinary drugs, fragrances, and cosmetics. Government agencies, such as EPA and European Water Framework, have proposed regulations to monitor water supply system. The analysis of contaminants in water, especially in drinking water, poses significant challenge due to low levels. Highly sensitive Agilent 6495 triple quadrupole LC/MS is the perfect tool to meet the challenge.
Method.
We have developed two methods to screen and quantitation of 140 PPCPs by dynamic multiple reaction monitoring (DMRM) with a total of 378 MRM transitions. The highly sensitive 6495 triple quadrupole LC/MS system is utilized to streamline the analysis by directly injecting 40uL water samples without analyte enrichment by solid phase extraction (SPE). The internal standards were kept at a constant concentration of 250ppt, while analyte standards were spiked at 10ppt, 25ppt, 50ppt, 100ppt, 250ppt, 500ppt and 1000ppt in reagent water. Three unknown samples were analysed in the presence of 250ppt internal standards.
Most of the PPCPs could be detected far below 10ppt, which was set as the reporting limit. Triplicates of spiked sample were injected for calibration curves. In most of the cases, the precision were excellent at each level. There were occasional cases that accuracy was beyond the 80-120%, with most of them close to 120% or 80%. Accuracy outliers occurred more in the 5-6 very hydrophobic compounds at lower levels due to their surface absorption to the vials. Correlation coefficients R^2 are greater than 0.99 for all the analytes except one (R^2 = 0.982) with quadratic fitting and 1/x weighting. For two of the three unknown samples, three PPCPs were found greater than 10ppt. More than 80 PPCPs were found in the third contaminated unknown sample.
Oral Presentation
Prepared by C. Marvin1, M. Murphy2, D. Yang3
1 - Agilent Technologies, Inc., 2850 Centerville Road, Wilmington, DE, 19808, United States
2 - EPA Region 8 lab, 16194 West 45th Drive, Golden, CO, 80403, United States
3 - Agilent Technologies, Inc., 5301 Stevens Creek Blvd, Santa Clara, CA, 95051, United States
Contact Information: [email protected]; 408-553-7091
ABSTRACT
PPCPs comprise a diverse collection of thousands of chemical substances, including prescription and over-the-counter therapeutic drugs, veterinary drugs, fragrances, and cosmetics. Government agencies, such as EPA and European Water Framework, have proposed regulations to monitor water supply system. The analysis of contaminants in water, especially in drinking water, poses significant challenge due to low levels. Highly sensitive Agilent 6495 triple quadrupole LC/MS is the perfect tool to meet the challenge.
Method.
We have developed two methods to screen and quantitation of 140 PPCPs by dynamic multiple reaction monitoring (DMRM) with a total of 378 MRM transitions. The highly sensitive 6495 triple quadrupole LC/MS system is utilized to streamline the analysis by directly injecting 40uL water samples without analyte enrichment by solid phase extraction (SPE). The internal standards were kept at a constant concentration of 250ppt, while analyte standards were spiked at 10ppt, 25ppt, 50ppt, 100ppt, 250ppt, 500ppt and 1000ppt in reagent water. Three unknown samples were analysed in the presence of 250ppt internal standards.
Most of the PPCPs could be detected far below 10ppt, which was set as the reporting limit. Triplicates of spiked sample were injected for calibration curves. In most of the cases, the precision were excellent at each level. There were occasional cases that accuracy was beyond the 80-120%, with most of them close to 120% or 80%. Accuracy outliers occurred more in the 5-6 very hydrophobic compounds at lower levels due to their surface absorption to the vials. Correlation coefficients R^2 are greater than 0.99 for all the analytes except one (R^2 = 0.982) with quadratic fitting and 1/x weighting. For two of the three unknown samples, three PPCPs were found greater than 10ppt. More than 80 PPCPs were found in the third contaminated unknown sample.
